Agent_Smith (Hive Bee)
07-11-01 00:55
No 189907
      OTC MDMA is now easy and cheap!!  Bookmark   

Welcome back bees.  It's amazing what you can do when you put your mind to it...  with the Hive gone, I've been forced to do a little research of my own.  So I researched, I tested, and I smiled, because there now exists an easy OTC synth of MDA, MDMA, MMDA, etc. without using RP of I2.  Behold How I made my first sucess!  (I wrote this write up for a friend w/o any chem knowledge, so its a bit basic.)

Agent_Smith's Easy OTC MDA synth:

Heres how this is going to work.  First, the safrole is going to halogenated.  Then, it's going to react with ammonia in order aminatate it into the lovely amphetamine derivative.  Boom, MDA.

The halogenation

The halogen you're going to use is bromine.  Fluorine is much to reactive to be safe with.  Chlorine won't work because it won't "mix" well with the safrole, needs a surfacant.  Bromine is easy to come by, cheap, and more reactive than iodine.  Iodine would work, but iodine salts are watched chemicals, and OTC iodine is expensive.  Also, iodine will require red phosphorus, which... sucks. 

Now, since we dont want to brominate the ring, were gonna use HBr rather than Br2.  HBr is a bitch to make.  I'll discuss quickly the ways of making it so that you don't feel compelled to find an easier way that won't work. 

NaBr is easily available OTC.  You can make HBr by reacting NaBr + sulphuric acid -> HBr + NaHSO4.  The problem is that HBr reacts with sulfuric acid to make Br2 (more like a sick solution of Br2 and a bunch of crap, but the key peice is that it doesn't make HBr).  NaBr and phosphoric acid should work, however, it requires heating under pressure to do so, which is impractical (heating at atmospheric will boil away the water before any HBr is released). 

 Thus, to generate the HBr gas we need to brominate the safrole NOT on the ring, we're going to brominate another aromatic ON the ring.  (Head spinning, ain't it?)

Ok, so, in order to brominate something on the ring (thus releasing HBr), we need Br2, which will be made by tearing the bromine out of NaBr (sodium bromide).  This can be done the same way that bromine is extracted from seawater (where NaBr exists in low concentrations).  The reaction is Cl2 + NaBr -> Br2 + NaCl.  Thus, we're going to gas a NaBr solution with chlorine in order to release bromine and table salt.

Chlorine will be made from pool shock (calcium hypochlorite) and muriatic acid (HCl)  Here's the procedure:

Making Chlorine

1) Make a chlorine gas generator.  Goto the hardware store and get 6 feet of 1/4" Polyvinyl tubing.  It's the small clear stuff.  Cut it into a 1 foot section and a 5 foot section.  One hose is going to put HCl in, the other is to take Cl gas out.  Now, cement, tape, expoy, or otherwise seal the two tubes into the neck of thebottle.  They should only eneter the bottle about 1 inch.  Find a syringe, at a local pharmacy.  Not a hypo. needle mind you, but just a syringe.  They can also be gotten at hobby stores.  Fit the nipple of the syringe into the 1 foot section of hose (you may need to use a different size hose, or tape things up to get a good seal. 

2) Goto the hardware store and pick up some powdered pool shock.  On the front of the package you'll find it's ingredients.  You want the highest percentage of calcium hypoclorite that you can find.  78% is the best I've seen, in "Super Sock It".  While you're there goto the cleaner's section and grab a liter or so of "Muriatic acid."  Chlorine is extremely toxic, it'd be a good idea to get a gas mask (not just a painters mask) while you're there.

3)  Fill the beer bottle about 1.5 inches high with powdered shock.  (This will require unsealing the hose from the bottle unless youre very patient and want to add it through the hose).

4) Now, fill the syringe with muriatic acid (HCl).  When you squeeze the syringe, the HCl will hit the shock and chlorine will come out of the longer hose.  You've got enough shcok in the to make a bunch of chlorine.  You'll have to refil the syringe about 10 times or so to use all the shock.  Stir the bottle before you unhook the syringe to refill it to make sure it's done reacting.

Now, using your chlorine gas generator you're going to gas a NaBr solution to release the bromine therein.  Theres a problem though.  Bromine is soluble in water, just like NaBr.  A bunch of the bromine is going to be lost into the water.  Also, bromine is liquid at room temp, but it's volitile.  That means it's going to make oodles of fumes, poisonous ones, so wear the gas mask that you should have bought by now.  In the future, you can cut costs down a whole bunch by finding something that NaBr is soluble in, but bromine is not.  I'm looking into this now, I'll let you know if I find something.  Here's how you'll make your bromine:

NOTE:  Apparently dropping H2SO4 onto a solid mixture of MnO (the balck stuff in Duracells) and NaBr will make bromine with the problem of loss into the water.  I haven't tried it though, but I have a feeling that it will work MUCH MUCH MUCH better than this.

Isolating Bromine

1)  Get Spa Bromine Base or Spa Brominator from Ace or Home Depot (Home Depot has it cheaper).  Make sure the ONLY ingredient listed (besides a few % inerts) is NaBr or sodium bromide. 

2)  Dissolve 40g of the bromine in 200ml (200g) of water.  You can use more if you want more bromine (you'll need a bunch, you'll have to do this many times, I'd proably do a large batch), but keep the NaBr to water ratio the same or even lighter on the water if you can get the NaBr to dissolve.  Don't use tap water for anything, use distilled. 

3)  Put the NaBr solution into a beaker or pitcher with a pouring spout.  This is important that the container has a spout, you'll see why in a second.

4)  Take the long hose for your chlorine gas generator and put it into the NaBr solution, and lay the hose into the pouring indentation/spout. 

5)  Take a large glass bowl, and fill it with ice water, very cold.  Put the bowl on top of the NaBr beaker.  The fewer gaps you have, the better.  You don't want to lose bromine to the air, but don't seal the bowl on, because the chlorine still needs to escape.

6)  Start slowly squeezing the syringe to produce chlorine.  The solution that was clear will turn orange, then red.  It will still be transparent.  After several minutes of gassing, the solution will turn cloudy red instead of transparent red.  I'm not sure why, but it seems that you don't gain anymore bromine after that point.  Let all the cloudy shit settle.

7)  Using a pipet (or a syringe) suck the black liquid off the bottom of the beaker.  Avoid grabbing any water.  Store this in a glass bottle with a plastic cap.  Don't use a rubber stopper or cap.  Don't use metal.

Making a Catalyst

Ok, that was the hard part, it gets easier now.  Once you've got about 50mls (150g) of bromine, you're ready to go.  I'm not taking the time to calculate exactly how much you'll need, but that should be enough to get a good yield from about 30g safrole.  Remember that bromination of an aromatic ring normally requires a catalyst.  Thankfully, iron reacts with liquid bromine to make FeBr3, and ideal Lewis Acid catalyst.  Get some Ultra Fine steel wool..  Get the finest you can.  Tear off about a gram and throw it into your bromine.  It might bubble a bit, but it will be dissolved into the bromine.  Now you're ready to make HBr and brominate your safrole:

Brominating Safrole

1)  Empty your Cl2 gas generator and clean it out. 

2)  Pop the bromine/catalyst solution into the bottle.

3)  Get some old fashioned mothballs.  You'll notice that they are nearly 100% naphthalene: perfect, an ideal aromatic.  Crush about 100grams of mothballs, not too fine though, leave it chunky.  You're going to add this is two additions, so divide it in half.

4)  Take the long tube from the gas generator and put it into a bottle of 30gs of COLD safrole.  Run the tube through a cold water bath before it reaches the safrole, this will cut down on how much bromine is released (It's not really a prob. but bromine is a volitile liquid).  It'd be ideal to have a bromine trap chmaber, but it is optional.  The ~30gram bottles of sassfrass work great as a container to brominate in.  Plug up the short tube, you're not going to use it.

5)  Throw in one half of the crushed mothballs and quickly seal the gas generator.  When the reaction stops completely, add the rest of the mothballs and seal again.

NOTE:  This reaction might give higher yields if it is conducted with the safrole dissolved in about 200ml of chloroform.  You can make that by getting a bottle of liquid pool shock from Ace, and popping it into a bucket with a full bag of ice.  Then add a cup of acetone (Acetone, not nailpolish remover),  Wait 30 minutes, and you'll have about 100mls of chloroform as an oily clear liquid at the bottom of the bucket.  Do that twice.

You now have bromosafrole.

The Amination

Kudos to Iudekx, this procedure is nearly verbatim from his OTC MMDA synth.

All you have to do now is react it with ammonia.  You'll need ammonium sulphate fertilizer.  This can be hard to find but it's readily avaiable at hardcore farm supply stores.  This will be reacted with sodium hydroxide (red devil lye, or some kinda of crystal drain cleaner, not Crystal Drano) to release ammonia gas.  HEED MY WARNING AMMONIA WILL KILL YOU FASTER THAN YOU CAN SAY "OOPS, THAT SMELLS FUNNY."  A store bought gas mask won't protect you from ammonia, you'll need to buy different cartridges for the mask to be safe.  The store might have ammonia proof cartridges, I don't know.  Heres what you have to do:

Methanolic Ammonia

NOTE:  if you want MDMA, you can make methylamine (good synth on rhodium's site) and put it in the methanol instead of the ammonia.  Yields will be better, but you'll have to invest in researching that on your own.

1)  Go get a mason jar.  Ask if you don't know what that is.  Get a bottle of gas line treatment, yellow bottle blue letters too.  That is methanol.

2)  Put the methanol into the mason jar, along with the long tube from the gas generator.

3)  Pop 140g ammonium sulphate into the gas generator bottle.  Dissolve 80g of lye into a bunch of water, but be wary that it can fit into the gas generator.

4)  Setup up the generator like you did for chlorine, and use the syringe to add NaOh and bubble ammonia into the methanol.  When all the lye has been added (might need to do 2 runs), pour in the bromosafrole, and seal tightly, VERY TIGHTLY.

Shake the jar every now and then for 7 days.  The longer you let it cook, the better yield you'll have.  You can heat it to speed up the reaction, but that will pressurize the bottle and it may explode... your call if its worth it.

After 7 days, carefully open the bottle, wearing your ammonia proof gas mask.   Then, do this to recover your MDA:

Extraction

1)  Grab your syringe and your HCl.  Fill the syringe with HCl, and slowly! drip HCl dropwise into the jar.  When the drops hit the jar, it will make a cloudy solid, ammonium chloride.  Add HCl until pH 2 or so (get test strips from any chemistry set).

2)  Filter the solution, discard the solid, and put the liquid on a large flat glass pan.  Put this out in the sun and wait for the methanol to evaporate (wont take long, methanol goes quick). 

3)  When all the methanol is gone, you'll be left with a powder covering the surface of your dish.  Guess what that is?

NOTE: it'd be a good idea to do a standard A/B extraction, this way is pretty dirty, but it works.

That's all I know.  Agent_Smith out.


blah blah blah something clever blah blah blah
 
 
 
 
    Rhodium
(Chief Bee)
07-11-01 01:05
No 189909
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

This method works all fine and dandy in theory, but what kind of yields can be expected in real life? I see that your post is lacking much detail, so I wonder, have you tried it out in practice, and what was your yield in each and every step?


http://rhodium.lycaeum.org
 
 
 
 
    Agent_Smith
(Hive Bee)
07-11-01 01:14
No 189911
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Yes, I tried it but once.  I've run into some trouble with the law of late, so I've decided to retire for a while, and won't be trying again soon. 

The run I did was around 70% in the halogenation (in chloroform) and 50% with a 12 day amination (ammonia).  I think 50% is the upper limit on ammonia aminations, if you want higher yields I'd use methylamine.  Also, for the whole process, if using chloroform and methylamine, I wouldn't expect anything over 70% (start to finish), with 80-85% yeilds possible with methylamine amination (based on others experiences).  The longer you gas in the first step, the better yields...

Still worth it if you ask me, all the 'cursors are so cheap.  The hard part really is the HBr, but I swear to god it works perfectly.

The bromine from the NaBr is the slopiest part.  You'll get only a few grams of bromine from 40g NaBr with the chlorine gassing in water (I tried this in a FBF with a reflux condensor as well, yields were no better).  Another solvent needs to be found, perhpas one where bromine is insoluble.  If I did this again, I'd use the NaBr and MnO mix + H2SO4 method to get the bromine.  Refs for that are everywhere, I dont have the eq'n offhand.


blah blah blah something clever blah blah blah
 
 
 
 
    Rhodium
(Chief Bee)
07-11-01 01:38
No 189913
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Acidify a concentrated NaBr (or KBr) solution with H2SO4, thereby getting aqueous HBr. Add H2O2 of any available concentration to oxidize the Hbr to Br2. You now have a dark red solution consisting of many things, but only the bromine is soluble in organic solvents like DCM, so just extract it from the aqueous phase.

It is a byzantine route to dry HBr you propose, but it is indeed creative.


http://rhodium.lycaeum.org
 
 
 
 
    Agent_Smith
(Hive Bee)
07-11-01 02:05
No 189918
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

byzantine indeed, but can you propose a better one?  I've tried em all, this one works.

Thx for the Br2 info, i didn't know it was the only thing that'd be soluble in organics.


blah blah blah something clever blah blah blah
 
 
 
 
    Rhodium
(Chief Bee)
07-11-01 02:14
No 189921
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

I am not experienced with OTC routes, as I do not know exactly what is OTC in the US. There are better routes to MDA, but they will normally use at least one precursor or reagent that is not OTC.

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    Agent_Smith
(Hive Bee)
07-11-01 02:22
No 189922
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Well, I thought it was worth posting for a few reasons, even though its not the best way to make MDA:

It is totally OTC, and probably OTC everywhere in the US

Unlike some other OTC routes, it doesn't require any tedious steps like stealing 80 bottles of I2 or scraping RP

The oxone method seems promising, but requires a bit of glassware, especially if the reduction is going to be done right.

So regardless, I consider it valuble, and for my situation, it was destined to be the perfect route.


blah blah blah something clever blah blah blah
 
 
 
 
    methadone
(Stranger)
07-11-01 06:35
No 189952
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

does the dmso method work?
Dmso+NaBr+oil==> bromosafrole???
 
 
 
 
    Agent_Smith
(Hive Bee)
07-11-01 06:59
No 189953
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Some (few) have said they made the DMSO route work, but it's my impression that the vast majority of people who try, fail.  Regardless, the DMSO rxn is indeed one thats highly sensitive to temp. and scale, and take a longs time. 

Thats another reason I feel this is valuable, it can be done on an afternoon, while the other methods (DMSO, oxone) require setups for many days.


blah blah blah something clever blah blah blah
 
 
 
 
    methadone
(Stranger)
07-12-01 05:21
No 190092
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

is there an easy way to make HBr gas from NaBr...and then just bubble that into glacial acetic acid ..like TS2 suggests..??
 
 
 
 
    Agent_Smith
(Hive Bee)
07-12-01 07:15
No 190100
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

wtf do you think the whole procedure here is doing (see paragraph 5)?  And don't use acetic acid, use chloroform.  better yet.. just follow the procedure.


blah blah blah something clever blah blah blah
 
 
 
 
    AMINATOR
(Stranger)
07-12-01 21:35
No 190191
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Yo! Agent smith! congrats to your Hbr method...you musta busted your ass cookin up that scheme, nice to see you...
anyway... here's a way to speed up your aminations and improve yields....

soak 40 bounce dryer sheets in a 32 oz. jar of methanol or isopropynol and shake well, for maybe 10 min. or leave overnight.
pour out the alcohol into a pyrexdish and ring out the bounce sheets then evaporate the alc. now scrape your quaternary ammonium sufactant from the pyrex evap dish while avoiding the scummy residue on the sides.
and voila!! your very own OTC quatenary ammonium phase transfer catalyst.  with this it might be possible to do a reasonable delepine reaction with hexamine or relativly kick ass reaction rates and yields for ammonia and definately kick ass yields for methylamine coolcoolcool maybe someone can think of a way to purify the PTC....if its ammonium salts I guess you could probably just do an A/B extraction...also you could probably get your bromo compound with the PTC and HCl gas and finkelstein style bromo-swap or for that matter Iodo-safrole. you can get KI/NaI from photography stores, salt licks.

Here's also a little inspiration for a NaI synth, though it would be probaly be easier to buy from a photo shop:

Powdered aluminum(flash powder)
I2 crystals
H2O
sodium hydroxide

Mix the iodine and aluminum powder intimately (Mortar and pestle) and anhydrously!!(will start fire with a drop of water and release HI and vaporous I2)It will probaly make a little HI gas while mixing due to air humidity and moisture in the aluminum powder(maybe dry Al powder in oven?don't use tincture I2 unless it is thouroghly dryed!!)

Now, heres the trick...hydrolysing the aluminum iodide to form HI. I don't know if you could pour the mixture slowly into the h2o to form it or reflux the shit added separatley to the water...but any way, once you made the hydroiodic acid all one needs to do is react sodium hydroxide to form sodium iodide and evaporate the water.

I just thought of this idea for a little inspiration this is not a tryed or tested method of producing NaI, every one.

Is there anyway of producing sodium metal from the hydroxide or chloride etc..or an otc source or maybe potassium? these metals would react vigorously to create NaI/KI. don't know how dangerous it is though.... ok I'm outa here
 
 
 
 
    BieneMaja
(Hive Bee)
07-13-01 21:37
No 190430
      Re: OTC MDMA is now easy and cheap!!  Bookmark   


Is there anyway of producing sodium metal from the hydroxide or chloride etc..or an otc source or maybe potassium? these metals would react vigorously to create NaI/KI. don't know how dangerous it is though.... ok I'm outa here



electrolysis of an NaCl/KCl melt. but there are only a few bees who are able to go this way. alkali + halogene always react *ipmressive*. there are more usable ways available.



ea vita est via in caelum (seneca)
[this life is the way to heaven]
 
 
 
 
    AMINATOR
(Stranger)
07-14-01 12:03
No 190521
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

I once heard of a "collision" reaction that involved gasing bromine with HI and it releases Hbr I wonder, if you made the aluminum Iodide and dropped small amounts in at a time in a solution of bromine and a hint of water, would it create Hbr gas? Maybe it would react slow enough to just dump it in?would this offer better yields of Hbr?
ahh maybe the aluminum would start to react with the bromine too....I don't know,just a thougt. hmmm.  ok how about this throw aluminum into slightly aqueous bromine and just let it make aluminum bromide that is hydrolysed by the water and makes Hbr in better yield. wudya think?...too exothermic? I wonder if the water would calm the reaction...
 
 
 
 
    AMINATOR
(Stranger)
07-14-01 21:34
No 190577
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Another thing that comes to mind, Agents Smith, is that if the sodium favors chlorine over bromine then why couldn't you drip hydrochloric acid on the NaBr to get your HBr. seams logical but I really don't know...I really like your sythesis idea and would only like to see it improve. I'd try this reaction myself but I'm flat broke right now. I appologise if it seams I am degrading your lovely procedure and all your hard work by suggesting different methods. I'm only trying to help.
 
 
 
 
    Rhodium
(Chief Bee)
07-14-01 21:55
No 190581
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Mixing hydrochoric acis with solid NaBr would create a solution, containing water, Na+, H+, Cl- and Br-. No HBr gas would be evolved, and certainly not anhydrous HBr gas, which is what we are looking for here.

The Hive - Clandestine Chemists Without Borders
 
 
 
 
    Agent_Smith
(Hive Bee)
07-14-01 23:16
No 190599
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

No no, aminator, feel free to suggestions.  I know my synth is... "byzantine"... but for me it was still hugely economical. 

I have, however, struggled with the NaBr and HCl idea a few months ago.  It makes lovely plume of white gas, but alas its HCl, with a very small amount of HBr mixed in.  It'd be sweet if that'd work though...


blah blah blah something clever blah blah blah
 
 
 
 
    Osmium
(Stoni's sexual toy)
07-15-01 01:10
No 190620
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

I suggest you all get a little more practical experience and some theoretical background as well. I don't see much viable useful information posted here. Simply throwing a few tidbits you heard about or saw in a chemistry book together will not provide you with a working synthesis for anything.
And don't throw all kinds of different syntheses and precursor preparation ideas into one thread, it gets way too cluttered, confusing and unreadable and after some time nobody will answer the questions anymore.

Sure Al and I2 will produce AlI3, but only a beginner would be brave (and stupid!)enough to mix them dry!
Adding anhydrous AlI3 to water will hydrolyse it, but you still end up with an aqueous solution of Al(H2O)6?I3 and only very little gaseous HI.
And sorry, I won't even comment on the suggestion of reacting alkali metals with elemental I2...

Don't try to reinvent the wheel, there are working syntheses for all these compounds around already. UTFSE, and don't clutter one thread with all kinds of different ideas, at least not when you want them being answered correctly and exhaustively.
 
 
 
 
    AMINATOR
(Newbee)
07-15-01 02:04
No 190630
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

O.k. I'm sorry, I guess maybe I'm a little over confident about my Ideas.All I have of chemistry knowledge, really is chemistry 20. I will be taking chem 30 next and eventually I will be enrolled in a chemical technology program. But I would surmise that its mostly because I love da Hive and beeing part of it. The Hive has sparked my interest in chemistry and thus it has been my decision to persue it as a proffesional career. Thanx everyone
 
 
 
 
    PolytheneSam
(Master Searcher)
07-15-01 02:49
No 190642
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Iodosafrole is supposed to be more reactive than the bromide according to some people.  I thought about this earlier, US patent 1380951 discloses a process for making HI from I2 using a terpene like pinene.  It sounds similar to the tetralin process.  Turpentine is mostly pinene.  Also, about the metallic sodium, I made some before using molten NaOH which is easily melted in an evaporating dish heated using a heating mantel or hot plate.  I used nails as electrodes and a 12V battery charger.  After a while little beads of sodium formed which I stored under mineral oil. 


http://www.geocities.com/dritte123/PSPF.html
 
 
 
 
    yellowjacket
(Hive Bee)
07-19-01 00:31
No 191601
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

One concern with this method in the past was the formation of other, non-desirable amines ("producing a scary and paranoid trip", to quote SOMM) during the amination process. Most writeups called for distilling the product after amination. Would the A/B get all the nasties out with this method?


marijuana is the flame, heroin is the fuse, LSD is the bomb!
 
 
 
 
    AMINATOR
(Newbee)
07-19-01 22:41
No 191884
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

my experience has been that when using single distilled oil. the halo-safrole will come out brown. My understanding is that pure-halosafrole is clear. brown stuff goes in, brown stuff comes out. Even after a/b you will end up with brown gak instead of crystals. The freebase must be distilled in order to get crystals. I would even distill the bromo before amination, so as that the brown nasties will not eat up all my amine first before maximum yield has been reached. as well as saving un halogenated safrol from being trashed and also interfering with the reaction.
 
 
 
 
    Agent_Smith
(Hive Bee)
07-20-01 00:05
No 191926
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

I didn't have problem with brown gak.  The oil did turn dark when the HBr was bubbled, however it's my experience that safrole darkens on exposure to most acids. 

The darkness effectively disappeared in the end product after an A/B was done on part of the product recovered by evap (the non a/b'd stuff looked a bit gunkie, off color). 

Also, as far as "nasties" are concerned, many sassafras oils are suprisingly pure safrole.  When I used to tinker with isomerization, it always boiled only a degree or two higher than pure safrole, which demonstrates relative purity, if not a precise measurment.


blah blah blah something clever blah blah blah
 
 
 
 
    Chromic
(Hive Addict)
07-20-01 00:49
No 191942
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Agent smith, that just means that your sassafras has got safrole. The impurities in sassafras will boil at a higher temperature than safrole. ie if you boil the sassafras down, it will boil at 232, then at 254, 280, etc.
 
 
 
 
    Agent_Smith
(Hive Bee)
07-20-01 03:11
No 191977
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Oh... I had myself convinced that the BP would change based on dissolved crap.  Now that I think about it, I feel like an idiot for posting that.  Oops.

Regardless, gunk was not a problem with my plain old sassafras oil.


blah blah blah something clever blah blah blah
 
 
 
 
    Agent_Smith
(Hive Bee)
07-20-01 03:20
No 191981
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

I've been toying with this, but haven't found OTC sources yet.  I think they exist, but I haven't seen em:

A more effcient way to make HBr might be to brominate tetralin (tetrahydronaphthalene) instead of naphthalene.  In my procedure, the bromine must be removed from water because if water is present, then the FeBr3 catalyst will form it's hydrate and work work.  Tetralin (to the best of my knowledge) will brominate wihtout a catalyst, which means that if it's added to an aqueous bromine solution, it *might* release HBr(g). 

I haven't tried this, because I haven't located OTC tetralin.  Tetralin is a turpentine replacement and may be found in a paint store.  Also, it's the major component of "Cuprex" a trademark referring to a pest/pediculicide that was also sold as a lice shampoo of the same name.  It seems to have gone off the market, so I dunno, but if you have an easy line on tetralin, that might work better for you.


blah blah blah something clever blah blah blah
 
 
 
 
    AMINATOR
(Hive Bee)
07-20-01 03:38
No 191987
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

I used Iodosafrole, I wonder if thats why...
did you get crystals after a/b?

 
 
 
 
    BieneMaja
(Hive Bee)
07-20-01 03:44
No 191989
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

afaik the synth via tetralin also uses iron dust as a catalysator, maybe yields are a bit higher but pure Tetralin won't be available otc, so naphthalene is the way to go.


ea vita est via in caelum (seneca)
[this life is the way to heaven]
 
 
 
 
    Agent_Smith
(Hive Bee)
07-20-01 06:26
No 192020
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Thanks for the info Biene...

That mean that nothign is to be gained by using tetralin, if it require a catalyst like you say, then the bromine canot be in solution.  Nevermind my previous post.


blah blah blah something clever blah blah blah
 
 
 
 
    BieneMaja
(Hive Bee)
07-20-01 15:26
No 192123
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

the ref i came across for HBr via tetralin uses a 2-neck rbf, in wich is tetraline and some iron dust, one neck is for an add. funnel dropping in Br2 the other one is the gas outlet, then comes the washing flask containing tetraline.. see other HBr thread. the only advantage tetralin has (maybe) is being liquid at room temp, so it is better mixable w/Br2.


ea vita est via in caelum (seneca)
[this life is the way to heaven]
 
 
 
 
    Agent_Smith
(Hive Bee)
07-20-01 22:24
No 192218
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Yeah, fi I could have found it, I probably would have used the tetralin.  I wonder, do you think the tetralin reaction could be used at lower temps?  If so, the flask could be cooled to reduce volatility of the bromine.  Bromine vapor was a minor problem with my naphthalene experiement, which seemed to work best at room temp or above.  I had to use a trap to ctach the bromine.


blah blah blah something clever blah blah blah
 
 
 
 
    BieneMaja
(Hive Bee)
07-20-01 23:44
No 192245
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

found the ref. again. from :
Houben-Weyl. Bd.5/4 (1960), S.18.
'[..]in the beginning, Br2 was added under  cooling [waterbath] [..]when the reaction slows down [..] [the mixture] is heated in the waterbath up to 30-40C. the washing flask filled with tetraline is used to hold bromine vapors back. the gas trap, cooled down to -60C, holds water, tetraline and last traces of bromine back.'

at what temp did u use your HBr generator? the setup used above is easyly built up with otc lab kit. one just has to lead his HBr through a kind of 'washing flask' loaded up w/ some more crushed naphthalene placed in a styrofoam box filled with crushed ice/NaCl or whatever. should help a lot, with the advantage over tetralin that the naphtha won't go with the HBr as it's mp is far higher than t.'s one making it much less volatile. was it that what you thought about?smile


ea vita est via in caelum (seneca)
[this life is the way to heaven]
 
 
 
 
    Agent_Smith
(Hive Bee)
07-21-01 00:09
No 192253
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

No, I hadn't thought about the volatility of the tetralin.  The naphthalene reaction proceeded with sufficient speed at room temp.  I was asking if the tetralin would proceed well at lower temp, thus eliminating the need for the trap or washing.  I see that this is not the case though, so I guess naphthalene was indeed the right choice.


blah blah blah something clever blah blah blah
 
 
 
 
    superhybrid
(Hive Bee)
07-21-01 05:06
No 192312
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

After the first page I didn't bother to read more. It is known that the halogen cation can be formed in a solution with Al halides and Fe halides. Which ones are for you to figure out.

For instance Iodine can be added to the benzene ring with AlCl3 as a reagent.

Here is the reaction

Benzene + I2-----AlCl3----->[I+ +  AlCl3I- + benzene]---->

Iodo benzene + HI  and the catylyst is rejuvinated.

This may work for other halogens and the methylene dioxy phenylalkene may be halogenated.
 
 
 
 
    Agent_Smith
(Hive Bee)
07-21-01 07:26
No 197803
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

I'm sorry, did your post contribute something?


blah blah blah something clever blah blah blah
 
 
 
 
    superhybrid
(Hive Bee)
07-21-01 20:05
No 197930
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Nope I guess I didn't did I.

Taking a week to produce a reaction is just too long in a closed system also for that matter. You may need a amine such as Et3NH3 to aid in the amination process. Don't hurt your self now.

What do we have here. I2, Br2, Cl2, F2. Which is more reactive or better yet which is more likely to come of the alkane in the amination procedure leaving the bare electophile to be snagged by the AMINE.

 
 
 
 
 
    Agent_Smith
(Hive Bee)
07-21-01 20:54
No 197944
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

In terms of the halogens themselves, I believe fluorine (and HF) is the most reactive.  However, in terms of the halogenation reactions, there seems to be a good portion of the Hive that insists iodine is more reactive than bromine.  I really don't know, I would have thought based on periodic trends that bromine is the more reactive...?

Either way, I used bromine since it's easier to obtain from 1lb bottles of NaBr (if I did it again I'd extract the bromine form the water into DCM and then form the catalyst in the DCM bromine mix) than iodine is to obtain from lots of bottles of tincture ($$).  Also, the bromine was liquid so it reacted easier with the solid naphthalene.  If using tetralin, then solid iodine would probably be fine, however making a catalyst for that reaction would SUCK since throwing some iron into a stack of iodine crystals is idiotic.  I think bromine is the way to go.

Chlorine is an option but I haven't done any experiments with it.  There are less references for chlorinations than brominations, but from what I understand a surfacant will be required when gassing with HCl (why?).  Aminator's technique for recovering quat. surfacants form dryer sheets might work for chlorination by gassing with HCl (although I suppose doing so will require distillation later on, the synth as is will probably end in gunk if the surfacants are not removed by distillation).


blah blah blah something clever blah blah blah
 
 
 
 
    improv_chem
(Hive Bee)
07-21-01 23:01
No 197961
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

I reciently found a source of iodine that is a 10.5% tincture which should give ~50g or more of solid Iodine for about $10.  Sure beats emptying out those tiny tincture bottles and makes Iodine a practical alternative.  I think the best way to extract it is to add NaOH solution with shaking until the iodine color goes away and then boil off the alcohol and water and whatever else until you have impure NaI.  Dissolve this in a minimium amount of water and vaccume filter off the insoluable crap to get a fairly pure solution of NaI.  You then just have to add some peroxide and HCl and you have your iodine.  Wash the  stuff with distilled water a few times and then do the usual methods to dry the iodine.  Anyways... The reason i brought this up was thinking about forming HI gas using I2 and red phosphorous from match strikers.  If one was to modify Iudexk's setup for OTC MMDA on rhodium's site to fill several ballons full of HI(g) and then slowly run the gas into the drying tube, then the suckback bottle, then into the Parsley leaf oil(or safrole or whatever) through a glass tube in a graduated cylinder (narrow and tall for max absorbtion).  You could also put some fiberglass wool over the end of the glass tube to increase absorbtion.  This really isn't new but mabe you could get away with using close to molar ratio's of HI and safrole if you could slowly release the gas from the balloons with a small plastic valve like those used for fish aquariums. 
The suckback bottle might not even be necessary if you already had the HI under slight pressure in the ballons....
Just something to think about....
BTW:  great write up Agent Smith! 
this one is getting copied and pasted in case the hive ever dissappears again!!
smile-improv


--Preventing odors from escaping to nearby noses is essential.....
 
 
 
 
    AMINATOR
(Hive Bee)
07-22-01 22:21
No 198119
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Agent smith, you are right, the flourine is the most reactive of the halogens and would probably hold onto safrole very tightly...what we want is a halogen that is not as strong, so as it will more easily leave the safrole in exchange for the amine.
 
 
 
 
    superhybrid
(Hive Bee)
07-22-01 23:03
No 198132
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Yeah ahem so which would it be then, Cl, Br or last but not least I. Hmmmmmmm.......
 
 
 
 
    Osmium
(Stoni's sexual toy)
07-23-01 00:09
No 198147
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Waaaah!
F2 is the most reactive of the elemental halogens, and I2 the least reactive. I2 doesn't react with aromatics anymore in the standard way, so iodobenzene production with Al or Fe catalyst won't work. Iodine won't react with aliphatic alkanes/terpenes either.
For the amination reaction iodosafrole works best, because iodide is the best leaving group. Fluorosafrole wouldn't work at all.

Read your chemistry books!
 
 
 
 
    Osmium
(Stoni's sexual toy)
07-23-01 00:17
No 198153
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

> I reciently found a source of iodine that is a 10.5%
> tincture. [...] I think the best way to extract it is to
> add NaOH solution with shaking until the iodine color
> goes away and then boil off the alcohol and water and
> whatever else until you have impure NaI.

This will produce NaIO, which will disproportionate into NaI and NaIO3. Once you acidify it again the reaction will go backwards, re-forming the I2. But you still have to add some H2O2 to take care of the iodide which was already present before you added the NaOH in the beginning.

> If one was to modify Iudexk's setup for OTC MMDA on
> rhodium's site to fill several ballons full of HI(g) and
> then slowly run the gas into the drying tube, then the
> suckback bottle, then into the Parsley leaf oil(or
> safrole or whatever) through a glass tube in a graduated
> cylinder (narrow and tall for max absorbtion).  You could
> also put some fiberglass wool over the end of the glass
> tube to increase absorbtion.  This really isn't new but
> mabe you could get away with using close to molar ratio's
> of HI and safrole if you could slowly release the gas
> from the balloons with a small plastic valve like those
> used for fish aquariums

I'm not convinced that this will work.
 
 
 
 
    Agent_Smith
(Hive Bee)
07-23-01 01:47
No 198168
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Tried it...  You'll have trouble filling the balloons.  The pressure in a P/P tank like the meth guys use is about all that reaction can handle, you might be suprised how much more pressure a balloon contains.  The balloons won't get very full, and then you'll have to deal with changing balloons (you're going to need a bunch, I'd say a balloon will only be able to hold about 2 liters with the pressure that reaction gives). 

And then theres the effects of HI on the rubber... I don't know if there are any, but it's a concern.

Hell, it might work, I don't know.  I do know that I hate scrounging for RP, thats why I came up with this.


blah blah blah something clever blah blah blah
 
 
 
 
    superhybrid
(Hive Bee)
07-23-01 06:27
No 198234
      Re: OTC MDMA is now easy and cheap!!  Bookmark   


I2 doesn't react with aromatics anymore in the standard way, so iodobenzene production with Al or Fe catalyst won't work.




For the production of iodobenzene one needs a metal chloride salt for the catalyst a iodine metal salt will not work for iodination. Don't make me whip out my org chem booksmile

 
 
 
 
    Osmium
(Stoni's sexual toy)
07-23-01 13:06
No 198297
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

>  For the production of iodobenzene one needs a metal chloride salt for the catalyst a
> iodine metal salt will not work for iodination. Don't make me whip out my org chem book

You need an oxidising agent actually, like HNO3.
Don't make me whip out mine...
 
 
 
 
    b159510
(Hive Bee)
07-23-01 14:34
No 198313
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

For the production of iodobenzene one needs a metal chloride salt for the catalyst a iodine metal salt will not work for iodination. Don't make me whip out my org chem book Yes, you should whip it out. And read it. As Osmium has said, nitric acid is used. You should have known this, being a second year chem major. Do you know why iodine is not added to the benzene ring the way chlorine and bromine are? After the posts I read in the novel forum, well... IMHO, nobody is really a chem major until after p-chem, and a little humility goes a long way, as I have learned ..Sorry, I'll go back to minding my own business now....

Back to the Primitive
 
 
 
 
    superhybrid
(Hive Bee)
07-23-01 14:34
No 198314
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

It was explained that the metal chloride salt formed the halide cation which would adjoin the benzene ring, Okay I get yasmile Yep it won't work sorry kid.
 
 
 
 
    yellowjacket
(Hive Bee)
07-24-01 01:26
No 198428
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Some renob tried Rhodium's route to bromine by acidifying NaBr with sulfuric and adding H2O2. This loser told me that the reaction is strongly exothermic, and will produce bromine gas.  Told him that he was a shit-for-brains and that bromine will choke your ass. Next time this dim bulb will try setting up a bubbler to catch the gas in a flask of DCM. He tried pouring some DCM over the reacting mixture, and noticed that it captured and held the bromine gas in solution quite effectivly. Also, icing down the rxn to keep the gas production down is on this doofus' mind also.  

marijuana is the flame, heroin is the fuse, LSD is the bomb!
 
 
 
 
    superhybrid
(Hive Bee)
07-24-01 04:12
No 198464
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Whoops indeed did some checking with Organic Chemistry by John McMurray and it was said that

Benzene + I2 ----CuCl2----> Iodobenzene (65%)

It was also stated that H2O2 woud also help the iodination as also HNO3 by another source. Had to do it didn't I.
 
 
 
 
    b159510
(Hive Bee)
07-24-01 04:20
No 198472
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

For the production of iodobenzene one needs a metal chloride salt for the catalyst The point is, you don't need it. Not 'can you use it'. Do you know why you don't need a metal catalyst?

Back to the Primitive
 
 
 
 
    b159510
(Hive Bee)
07-24-01 04:24
No 198473
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Nevermind, answer it if you want. Or not, I don't care.
Sorry for crapin on your thread Agent.

Back to the Primitive
 
 
 
 
    superhybrid
(Hive Bee)
07-24-01 05:07
No 198492
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

It would seem to me that this thread has gotten way off course. I always like to scrap with Os though hehe.
 
 
 
 
    swic
(Stranger)
07-26-01 08:16
No 198993
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

I just wanna add- Methylamine from hexamine STINKS!!! Thank you all!

http://www.pot-tv.com
 
 
 
 
    baalchemist
(Hive Bee / Eraser)
07-27-01 09:10
No 199239
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

What do you mean by cheap and easy now?, Doesnt sound too simple of a task. Baals cost to make Ketone runs ~.17c/gram
 
 
 
 
    Agent_Smith
(Hive Bee)
07-27-01 18:16
No 199341
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

What seems expensive.  Save for the safrole, this doesn't use any chem that can't be had for a dollar a pound. 

And easy is refers to the fact that theres much less ambiguity than in the established methods.  You set this up in an afternoon, by 5 oclock youll know if you did it right.  Non of the 48 hour relfuxes and watching for color changes.  Regardless of that, theres still less steps than a typical ketone / reduction.  Also, no RP like other OTCs

blah blah blah something clever blah blah blah
 
 
 
 
    foxy2
(Hive Addict)
07-29-01 13:29
No 199737
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Agent

Have you succeeded in making anything with this method?

Buy that reply I would say Not.

Nothing is done that fast, maybe after many trials when you have the procedure down, but not initially!

Do Your Part To Win The War
 
 
 
 
    Agent_Smith
(Hive Bee)
07-29-01 18:09
No 199780
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Even if you were trying to take forever, theres really no way you could stretch this out to more than a one day operation.

Yes, I have achieved honey this synth, my yields are posted at the top of this thread.

blah blah blah something clever blah blah blah
 
 
 
 
    foxy2
(Hive Addict)
07-30-01 10:38
No 199974
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Yea so how much did you have at the end of the day??
Weight? 
tongue

Do Your Part To Win The War
 
 
 
 
    baalchemist
(Hive Bee / Eraser)
07-30-01 11:56
No 199986
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Says he started with 30g's of safrole, cant imagine more than 25g's tops coming out. Thats not too much dope for an afternoons work, I would think an easy one like this could pump 100g+ at least in an afternoon.
 
 
 
 
    Agent_Smith
(Hive Bee)
07-30-01 19:29
No 200054
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

My yield was around 29g of bromosafrole, ~70%

As I said before, yield in the amination was poor, about 50%, giving me somewhere around 10g of goodies.

blah blah blah something clever blah blah blah
 
 
 
 
    naturalblonde
(Stranger)
08-06-01 07:56
No 201742
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

> 4)  Setup up the generator like you did for chlorine,
> and use the syringe to add NaOh and bubble ammonia into
> the methanol.  When all the lye has been added (might
> need to do 2 runs), pour in the bromosafrole, and seal
> tightly, VERY TIGHTLY.

Agent Smith, I totally like your OTC approach to life, even if it means sacrificing some yield. Good rules to live by.

No disrespect intended, but have any of your friends actually gotten the amination to work?

I don't fully understand the physical chemistry involved, but most chemical ammonia generators I've heard about don't really like to politely bubble NH3 into a solution in a closed system. Instead a backpressure seems to form and sucks the solution right back into the generator.

The ancient high-school colored-water/ammonia fountain is an example of this phenomenon.

Opinions? Ideas?

 
 
 
 
    Ghost_Of_BT
(Newbee)
08-06-01 19:55
No 201870
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

The NH4 will bubble through methanol for a while before it starts sucking back. So just whip out the tube when it starts sucking.

Visit www.the-hive.ws
 
 
 
 
    Agent_Smith
(Hive Bee)
08-08-01 00:01
No 202297
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Suck back on the ammonia reaction is not as bad as some I've seen.  It can be a problem, check valves or such can help.  Personally I just whip the hose out like BT suggested.

Yes, it does work as described, I've posted yields.

blah blah blah something clever blah blah blah
 
 
 
 
    obituary
(Hive Addict)
08-08-01 02:00
No 202334
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

forget the valve, take and find a way to get a plain glass funnel into your gassing chamber- yes, you might have to change the chamber your currently using to accomodate- anyway, run the hose in, attach the hose to the funnel and lower it into the solution by about a 1/4 inch, this will allow the gas to bubble through, but when the suckback occurs, it can only draw so much liquid before the the vacuum is broken, self regulating.  maybe not the most sophisticated of apparatus, but it does work.

 
 
 
 
    tomjuan
(Hive Bee)
08-10-01 03:32
No 202987
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

So to recap your procedure, as well as add Rhodium's suggestion for making Br2, is this what we have?

halogenation
------------
Add sulfuric acid to sodium bromide (NaBr) to produce aqueous HBr acid
Add H2O2 to this mixture to produce Br2
Extract the Br2 with organic solvent like DCM
Add a small amount of iron to make some FeBr3 as a catalyst
Add naphthalene (mothballs) to the FeBr3/Br2 solution to produce gaseous HBr
Gas safrole to produce bromosafrole

animation
---------
Add NaOH solution to methylamine HCl to produce methylamine gas
Gas methanol to  produce methylamine/methanol solution
Add the bromosafrole to the methanol/methylamine
Seal the container, and shake occasionally for seven days.

extraction
----------
Do a full A/B extraction, recrystallization, etc...
-OR-
Acidify the rxn product to pH 2.
Filter out any solids
Evaporate the methanol away
Hope for the best as far as purity is concerned . . .
 
 
 
 
    Rhodium
(Chief Bee)
08-10-01 14:11
No 203122
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Make sure you separate all the DCM from the bromine before adding it to naphtalene/FeBr3, or you will perform a friedel-crafts alkylation/polymerization with the naphtalene.
 
 
 
 
    Osmium
(Stoni's sexual toy)
08-10-01 15:07
No 203132
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

DCM is surprisingly inert in Friedel Crafts reactions, Ive even used as a solvent for such reactions (with AlCl3 and acetyl chloride).
 
 
 
 
    Rhodium
(Chief Bee)
08-10-01 15:13
No 203133
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Have you? On what substrates? Both methyl chloride and chloroform is reactive in such conditions.
 
 
 
 
    tomjuan
(Hive Bee)
08-10-01 15:53
No 203138
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Would there be a less reactive solvent I could use for the Br2 extraction? Or is there a way to separate the Br2 and DCM without distillation? One good thing about this synthesis (if it could really be made to work with satisfactory yields) is that it doesn't require distillation or reduced pressure.
 
 
 
 
    Rhodium
(Chief Bee)
08-10-01 16:12
No 203145
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Diethyl ether should work.
 
 
 
 
    tomjuan
(Hive Bee)
08-10-01 16:28
No 203147
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Hmmm. Diethyl ether isn't exactly over-the-counter, although making it isn't that hard. Posts like this raise a little warning flag me. They might lead someone to believe they can just follow the indicated procedures and produce something safe and effective without knowing anything at all about the chemistry behind what they are doing.

I think I know someone who might try this synth in the next few days, and do a real write up on the results complete with yields and better physical descriptions of the appearances of the intermediate products.
 
 
 
 
    goiterjoe
(Hive Addict)
08-10-01 17:15
No 203155
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Diethyl ether is the stuff in starting fluid.  You shouldn't have any trouble finding it at the auto parts store. 

Drunk driving, that's what I like to do,
I like drunk driving with you.
 
 
 
 
    tomjuan
(Hive Bee)
08-10-01 18:01
No 203161
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

The only types of starting fluid I can find around here have significant amounts of impurites, like heptane and ether-soluble lubricants. I have tried doing the water washing, but what I end up with doesn't even SMELL like ether. I certainly haven't given up on this route yet - I am still keeping my eyes open for new brands I haven't tried.

Regarding DCM, the separation of DCM (bp 39C) and bromine (bp 58C) is 19 degrees C. What would be the likely outcome of trying to evaporate away the DCM over a regular heat source without a column? Also, there was a claim that DCM wouldn't react and there might not be a need to separate the bromine after all - was there ever a verdict on this?
 
 
 
 
    b159510
(Professional Student)
08-10-01 20:16
No 203182
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Regarding DCM, the separation of DCM (bp 39C) and bromine (bp 58C) is 19 degrees C. What would be the likely outcome of trying to evaporate away the DCM over a regular heat source without a column? I imagine the result would be incomplete separation. Br2 rapidly evaporates at room temp where I live. A fractionating column should be used for volatile chemicals with a difference in bp less than 40C.

Back to the Primitive
 
 
 
 
    Rhodium
(Chief Bee)
08-10-01 20:17
No 203183
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

You can NOT evaporate away DCM from bromine, you would need to fractionally distill with good ventilation.
 
 
 
 
    tomjuan
(Hive Bee)
08-10-01 20:34
No 203196
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Yeah, that's what I figured - thanks for your answer.
 
 
 
 
    jacob019
(Stranger)
08-14-01 19:31
No 204480
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Is distillation the only way to get the safrole out of the sassafras?
 
 
 
 
    Osmium
(Stoni's sexual toy)
08-14-01 20:17
No 204500
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Freezing works too. UTFSE.
 
 
 
 
    jacob019
(Stranger)
08-15-01 03:40
No 204639
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

How exactly would that work, does the safrole freeze and you just filter it out or does the other stuff freeze and your left with safrole.  What should the temp be taken to? And is isolating safrole realy necessary. Could you just use sassafras oil raw?  Sorry to be so inquisitive, but answers would make a good start for this recipe.  Thanks again.
 
 
 
 
    Osmium
(Stoni's sexual toy)
08-15-01 06:49
No 204688
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

> does the safrole freeze and you just filter it out or
> does the other stuff freeze and your left with safrole.

The safrole will freeze first, it has a melting point of about 11C when pure. 

> What should the temp be taken to?

Below the melting point of safrole. Freezer temps.

> And is isolating safrole realy necessary. Could you just
> use sassafras oil raw?

Depends on what synth you wanna perform, safrole content of your oil etc. It surely doesn't hurt to distill it.

> Sorry to be so inquisitive, but answers would make a good
> start for this recipe.

UTFSE. All this stuff has been talked about countless times in the past.
 
 
 
 
    Bwiti
(Hive Addict)
08-15-01 16:16
No 204764
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

"The only types of starting fluid I can find around here have significant amounts of impurites, like heptane and ether-soluble lubricants."

  Here's what works for me: Spray into a pipe and dribble the impure ether into a flask. Distill this into a jar that's in ice. Wash the ether with distilled H2O. Bake the H2O out of some epsom salts in the oven and use this to dry the ether. Sure, the ether will probably still have some hydrocarbons left in it, but beggars can't be choosers.
  Would sulfur convert the bromine to HBr? Peace!tongue

  I'm going to help all of you cleanse this diseased planet.
 
 
 
 
    Agent_Smith
(Hive Bee)
08-15-01 21:52
No 204860
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Check out the text on rhodiums site about HI.. it has some info on making HX with sulfur...  I remember looking at it, but if memory serves, it was for producing the aqeuous acid...?

blah blah blah something clever blah blah blah
 
 
 
 
    Agent_Smith
(Hive Bee)
08-28-01 00:14
No 207802
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

What the hell?  Someone's rippin' off my shizatt:

http://www.voy.com/12987/464.html

What is that place?  A Hive for squinty-eyed bees?

blah blah blah something clever blah blah blah
 
 
 
 
    AMINATOR
(Hive Bee)
08-28-01 05:13
No 207887
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

your famous!!!!has anyone tried the reaction with a surfactant? Agent smith?....squinty eyed beez ha ha!!laugh
 
 
 
 
    halfapint
(Ubiquitous Precursor Medal Winner)
08-28-01 05:36
No 207895
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

More about the amination a la IudeXK, pleez. Bromosaf in a jar full of methanolic ammonia and forget it for a while. More action, the public demands. Let's have a glued PVC pipe bomb wrapped in a wad of duct tape and nuke it in the wave.

turning science fact into <<science fiction>>
 
 
 
 
    AMINATOR
(Hive Bee)
08-28-01 07:23
No 207917
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Now your talkin'!!... why didn't I think of that?? how about one of those scew in cap ends. Or how about a home made reflux apparatus adapted inside a microwave? made of acrylic plastic tubes and epoxy. I cant wait!! me thinks the war is most definatley over!!! this is getting easier and easier.
 
 
 
 
    Agent_Smith
(Hive Bee)
08-28-01 15:46
No 207999
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

PVC isn't a good idea.  It release some nasty ass shit when heated.  I'm not sure if the temperatures in the nuker would be high enough to cause problems, but heating plastic pipe under pressure doesn't sound kosher.  I'd use steel.

The amination ala Iudekx can be found on Rhodium's site, mmda.txt, under the heading "OTC MMDA from Parsely Oil" or something like that.

I don't understand why everyone here has so much trouble with microwave apparati.  If you're gonna do some nuking in your dreams, make a reflux apparatus for your microwave.  Despite popular belief, you don't need to cut holes in your nuker.  Try this instead:

Locate the wave source in your microwave.  Usually, the wave source is a 12" diameter disk seen in the top of the cooking chamber (in here is a big metal propeller than spins and help distribute waves).  Now, there should be some room on either side of the disk (if not, you can use an area underneath it.  Take a peice of metal with no holes larger than a few millimeters, and use to to block off a section of your microwave.  The wave source should not be located inside this new chmaber, the shield must be between the walls of the nuker and the wave source.  Now, grab a bukcet of ice, and stick it in the new chamber.  For your reaction "Flask" get some microwave safe container, and rig it with some hose coming out of the top, and returning to the bottom.  Place the flask in the main microwave chamber, with the hose running into your shielded chamber and through your bowl of ice.  Voila, instant reflux condensor. 

Alternatively, you can go here http://www.randf.com/matc.html and buy some nuker shieding instead of the metal shield.  Both will block microwaves, but for the skeptics...

The ice will melt eventually, but the shielding will be sufficient to prevent that for long periods of time.  Nothing says you can't pop open the microwave and put more ice in though, and a good supply of ice should last a while.  Fiberglass insulation can be added to further buffer you ice chamber fomr the nasty nuker.


blah blah blah something clever blah blah blah
 
 
 
 
    AMINATOR
(Hive Bee)
08-28-01 16:51
No 208010
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

here's another thought get a piece of duct sheeting and cut a hole in it and turn your microwave on it's back. open the door and somehow defeat the safety mechanizm then mount your metal sheet over the opening. now you don't have to cut a hole in the top. I've just decided that refluxing with ammonia will loose all your ammonia I think...sounds to much like the preparation of liquid ammonia page on Rhodium's site. maybe you could use dry ice acetone through the condesor but what a pain in the ass!!! methylamine hcl should be fine wonderwhat hexamine does in the microwave???
 
 
 
 
    Gen_Washington
(Hive Bee)
08-31-01 02:29
No 208809
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Agents_Smith, great post!

~Your ~50 ml of Br2, how much HBr gas did it produce, or how long did it produce gas?

~In SOMM5, the Univ of Alabama (??) had a tank of HBr gas and/or somehow used 70% HBR acid, "a quite uncommon reagent"

How long did they gas for, and what were their yields?
 
 
 
 
    Agent_Smith
(Hive Bee)
08-31-01 04:32
No 208836
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

50mls of Br2 will gas for a looooong time. The amount of time can be changed by the amount of naphthalene and more importantly the amount of catalyst.

I hadn't looked into that Alabama ref.  Whenever I read things about people with HBr cylinders, I get jealous and angry and break things...

I've been getting a few PMs about people with tar problems.  The tar is because while the HBr brominates the safrole, it also fucks some of it up (I think the MD bridge is cleaved or something).  In my experience, tar is exponentially less of a problem if the sassafras is in chloroform...

blah blah blah something clever blah blah blah
 
 
 
 
    amalgum
(Stranger)
08-31-01 21:07
No 209064
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Dude, I have been writing synths like this for about a year now.
Exceot mine were using NaI or KI (liberated from salt licks)
with sulfuric acid to produce HI, wich is bubbled slowly through a DCM/safrole solution. 
The solution is then washed a few times with dilute NaOH, and the DCM stripped.
The resulting iodosaf can be aminated in the way yo suggest.

Oh yeah, and ammonium sulfate can be made from those dilute household ammonical solutions, and then reacted with NaOH the free NH33 gas.
That is so OTC that I'll smack myself.
 
 
 
 
    TheCuriousOne
(Stranger)
08-31-01 22:00
No 209085
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Hello! Im new here! (can't ya tell?):)
This thread is really quite interesting...
Im curious - would subbing myrsiticin for safrole in this process yield MMDA?  If not, why wouldnt it?
Thanks for listening - I never knew chemistry could be so fascinating.

TCO
 
 
 
 
    Rhodium
(Chief Bee)
08-31-01 22:57
No 209115
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Yes it would. Look at ../rhodium/chemistry /mmda.txt
 
 
 
 
    terbium
(Hive Addict)
09-01-01 04:14
No 209199
      Re: OTC MDMA is now easy and cheap!!  Bookmark   


Dude, I have been writing synths like this for about a year now.
Exceot mine were using NaI or KI (liberated from salt licks)
with sulfuric acid to produce HI,



I am guessing that you have never actually tried this.

 
 
 
 
    TheCuriousOne
(Stranger)
09-01-01 07:14
No 209233
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Thanks for the link, Rhodium!  So much to learn...So subbing elemicin would yield TMA with this process, then?
If the proper reactions were followed using myristicin, but mythalamine or elemicin was used in the amination step, what compound would be the result?  Its going to be a bit before I can answer that one myself:)

TCO
 
 
 
 
    Agent_Smith
(Hive Bee)
09-01-01 08:08
No 209239
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

amalgum, those synths you've been writing will not work, sorry

such things have been posted all over the hive

blah blah blah something clever blah blah blah
 
 
 
 
    amalgum
(Stranger)
09-05-01 05:44
No 210202
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Why not?  The whole thing is to creat HX gas, and introduce it to the safrole.  If this is done, why wont the halogenated product work?
 
 
 
 
    Agent_Smith
(Hive Bee)
09-05-01 06:59
No 210226
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

you putz, do u think I wrote this long synth for HX gas for my health?  You can't use H2SO4 to make HX, the H2SO4 will oxidize any HX to X2.  ALso, you won't get much, if any NaI or KI from a salt lick.  Finally, DCM is a shitty solvent for the gassing, only DMF and CHCl3 have referrences showing that they inhibit cleavage. 

So, yeah, basically, evenything you've been writing is wrong.

blah blah blah something clever blah blah blah
 
 
 
 
    improv_chem
(Hive Bee)
09-05-01 21:14
No 210421
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

The Source for 10.5% Iodine does indeed produce Iodine in this way but like you pointed out Acid and H2O2 are needed to convert the solution of NaI back to elemental Iodine.  The amounts don't have to be exact, as two shot glasses one of HCl and the other of 3% H2O2 will convert several grams of Iodine. 
I realized after i posted that I hadn't really read over Agent_Smith's method very well and didn't see the obvious benifits over the phosphorous method to make HI. 
Sorry about the delay since my last posting, I've been the wilderness searching for botanical sources of certain substances!
I should be around more now that i'm back in civilization once again.wink
-improvsmile

Let's play with nature a little, I'm sure we can make her a little higher....
 
 
 
 
    Gen_Washington
(Hive Bee)
10-04-01 04:31
No 220073
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

#1  Ratios of NH4SO3 (?) to make NH3 w/ lye:  are the amounts based on some scientific equation, or actually fertilizer since Mr Clean points out, and looks like to me, the fertilzer is about 15% sulfate?

#2  THE GOO:  Might bee form heat, look at Festers book.

#3  Speaking of:  Saw book other night, sez use ice bath, not even stirplate heat alllowed, and used 200ml glacial acetic/200 ml sassy oil (undistilled, I presume).  What do various experts (and sexperts) think around here?:  given little resources/time, better of with choloroform, DMF, or glacial acetic?  ({Please rate in order, send check/money order, phone, zip, SS#, checking acct#, & all PIN #'s too)NOW)
 
 
 
 
    Agent_Smith
(Hive Bee)
10-04-01 20:49
No 220310
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

#1  I didn't calculate the stoichimetric ratios.  I stole that bit from Iudekx, I know it works, but stoichiometricly it might very well be wrong.  Balance equations and finding molecular weights is so boring....

#2  Nope, its fairly well established that goo is from MD clevage.  The colder the temp, the less cleavage, so indirectly, I suppose it's related.

#3  You are most ceratinly better off with DMF or chloroform than GAA.  Theres a post in Serious Chem.  "Bromosafrole Breakthrough" that in clear referenced terms says that GAA does dick to inhibit MD cleavage and that solutions in DMF were shown to be stable for several hours.  Osmium made the deduction that chloroform would be comparable to DMF, my experiments seem to indicate hes correct.  Hell, chloroform is easier to get that GAA anyway, so why bother with acetic acid?

blah blah blah something clever blah blah blah
 
 
 
 
    jacob019
(Stranger)
10-08-01 17:52
No 221675
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Forgive me for being rude, but would it be possible to just pump chlorine gas through safrole to produce chlorosafrole in any reasonable yeild? I know it works with isosafrole for the dichloro derivitive.  Could the chlorosafrole be reacted with methylamine directly? With or without heat?  I know yeilds would be worse, but I'm not finding NaBr.
 
 
 
 
    Rhodium
(Chief Bee)
10-08-01 17:54
No 221676
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

No, bubbling chlorine gas through safrole would yield 1-(3,4-methylenedioxyphenyl)-2,3-dichloropropane ("dichlorosafrole"), which I don't know of any good use for.
 
 
 
 
    jacob019
(Stranger)
10-08-01 19:43
No 221714
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

I thought the route to the dichlorosafrole was done by pumping chlorine gas through isosafrole not safrole.  The dichlorosafrole can then be refluxed with KOH to produce MDP2P in 60% or so yields.  If I can produce the dichlorosafrole straigt from safrole, that would make my life much easier.
 
 
 
 
    Lem2
(Hive Bee)
10-08-01 21:04
No 221753
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

do you have refs for this? it would definately be most kewl if that would work.laugh

Maybe Safrole w/ HCl bubbled through it w/ PTC to form chloro safrole, then a reflux w/ [K/Na]OH?
 
 
 
 
    IudexK2
(Stranger)
10-08-01 21:14
No 221759
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

What about:

safrole + Br2 ---> dibromosafrole
dibromosafrole + KOH ---> MDP2P

Does this really work? Surely I'd have heard about it before if it did...

Sweet dreams,
IudexK
 
 
 
 
    jacob019
(Stranger)
10-08-01 21:26
No 221766
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

It has been descussed, search.  I know the procedure works, what is PTC?  I'm going to dream with the whole idea this week, I'm planning on using chlorine gas, but that sucks and HCL would be tight.  All the procedures for the dichlorosafrole use isosafrole.  The question is can I just use strait up safrole.

another Idea I had was puting bromosafrole through the Al/Hg with nitromethane.  The reflux conditions and methylamine would be there, but would the reaction have an affect on the bromosafrole other than it's reaction with the methylamine.  It would be really cool if this would work because bromosafrole would then just be like a lower yeilding MDP2P.  That would be OK though because I'd save the yeild lost in the reactions that I would use to get MDP2P. The whole dichlorosafrole to MDP2P thing yeilds not much more than 50-60% from the safrole.
 
 
 
 
    Agent_Smith
(Hive Bee)
10-08-01 21:33
No 221771
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Never heard anything about that KOH reflux to MDP2P, it'd be nice though.

I've seen refs for the HCl + safrole + PTC --> chlorosafrole reaction.  You will most likely indeed get chlorosafrole form such a reaction.  I'm not sure exactly which PTC to use those, or if it'll be OTC.  The only problems I might forsee is that the chlorine may be too sticky, i.e. it'll bond to the safrole too tightly for a room temperature amination to work.  I think the only way to aminate chlorosafrole would be a bomb type thing.  ...??

blah blah blah something clever blah blah blah
 
 
 
 
    IudexK2
(Newbee)
10-08-01 22:07
No 221791
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

yep, chlorosafrole is not readily aminated enough for a room temp. amination to bee useful.
 
 
 
 
    IudexK2
(Newbee)
10-08-01 23:59
No 221854
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

ok, so dihalogenating a propenylbenzene and then refluxing it with KOH will yield the phenylacetone, albeeit in not very good yields. However, I think this would only work with isosafrole, not safrole.

PTC = phase transfer catalyst

Sweet dreamz,
IudexK
 
 
 
 
    IudexK2
(Newbee)
10-09-01 00:19
No 221862
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Rhodium? Are you sure safrole + Cl2 ---> dichlorosafrole? This seems ridiculously easy... why do ppl bother with p-benzoquinone etc. if all it takes is a halogen and KOH!??
 
 
 
 
    Osmium
(Stoni's sexual toy)
10-09-01 00:36
No 221867
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

The halogens will be in the wrong locations. You have to use isosafrole.
 
 
 
 
    jacob019
(Stranger)
10-09-01 02:10
No 221907
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Question about the agents original procedure...
Why can't bromosafrole be refluxed with methylamine.  Why bother with the whole week long deal.  Would the methylamine not condense and just be driven off as a gas?  If thats the problem would a bomb work?  And would Fe/HCl hurt the bromosafroleIf thats the problem would a bomb work?  Could nitro+bromosafrole+Fe/HCl simply be bombed to get the goodies?
 
 
 
 
    Agent_Smith
(Hive Bee)
10-09-01 03:13
No 221946
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Sure, MeAm reflux will work fine.  MeAm bomb will work fine too.  Probably even work better. 

I doubt that Fe HCl nitromethane and bromosassy in a bomb will do anything for you.

blah blah blah something clever blah blah blah
 
 
 
 
    jacob019
(Stranger)
10-09-01 03:51
No 221959
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

from elusis' methylamine faq
Assemble a 500mL RB flask with claisen adapter, thermometer down the center to read the liquid temperature, and reflux condenser with a cork and tube leading to a beaker of 1M Hydrochloric acid. Drop a stirrer magnet in, then add 105g of 40 Mesh Iron filings, 225mL of water and 1g of Ferric Chloride. Next, add 35mL of concentrated Hydrochloric Acid ("muriatic acid" is ok). When the bubbling ceases, add 31g of Nitromethane.

Heat the reaction mixture to 100C and hold for 14 hours. A temperature regulator is necessary if using a heating mantle, else use a large boiling water bath (if you will be doing it overnight, so it doesn't run out).

All that is going on here to convert the Nitro to Methylamine is Fe, FeCl, HCl, and Nitro being heated to 100 so that part would work I don't see why bromosafrole would interfere with that reaction.  The resulting methylamine would react with the bromosafrole given reflux conditions.  So where's the problem?  Only one I can see would be the Fe or HCl interfering with the bromosafrole + methylamine reaction.  This reaction would be a little bit similar to the Nitromethane Al/Hg.  Think of how easy it would be.
Safrole + HBr --> bromosafrole
bromosafrole + Fe + HCl + nitromethane --> MDMA
I'll try it this week unless you can give me a good reason not to.  Please comment.
 
 
 
 
    Agent_Smith
(Hive Bee)
10-09-01 06:23
No 222046
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Ferric chloride is FeCl3, not FeCl or FeCl2..  you didn't mention using it in your post, so were you planning that Fe and HCl will form the FeCl3 in situ?  That is your flaw.

If you've got FeCl3 laying around then it might work excellently.

blah blah blah something clever blah blah blah
 
 
 
 
    IudexK2
(Newbee)
10-09-01 10:12
No 222147
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

SWIM has a feeling that if conducted at high temps as in bomb, this rxn will produce unwanted side-products which do not occur or occur to a much lesser extent if done at room temp. FeCl3.6H2O is available cheap form electronic supply places for etching.

So, am I to understand that if you add a halogen to a propenylbenzene, and reflux the formed dihalo- derivative with KOH, you will get the phenylacetone? If this is true, the implications for clandestine chemistry are staggering! laugh

Sweet dreams,
IudexK
 
 
 
 
    jacob019
(Newbee)
10-09-01 16:41
No 222243
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Can the FeCl6.H2O be used directly or does it need to be heated to remove the .6H2O?  What if instead of a bomb, I just refluxed?  Elusis' post says to bring it to 100 maybe I could take the mix there for a while, and if it's not a good reflux take it up after the methylamine has been formed.  Ohh how fun.  Yes, the dihalo thing is cool.  I wonder if I could just mix Br2, with the isosafrole to get the appropriate dibromo compound.  Hmmmmm... wink
 
 
 
 
    Rhodium
(Chief Bee)
10-09-01 17:48
No 222276
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Iudexk: Yes, that is the implications of the japanese journal at the top. If someone could find the primary reference for this, we would all be grateful.

Why is there no japanese/chinese speaking bees on this board? You account for 20% of the world's population!
 
 
 
 
    SANREMI
(Stranger)
11-02-01 21:48
No 232234
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

the choice of a solvant can give your reaction some drection, i think
could ethyl ether be use as chloroform?
 
 
 
 
    Agent_Smith
(Hive Bee)
11-02-01 23:14
No 232254
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

::beats head against wall:: NO GODDAMNIT.. CHCl3 or DMF, read the %@#$^%@#$ post!

blah blah blah something clever blah blah blah, email at dateline@nbc.com
 
 
 
 
    dr0k
(Stranger)
11-08-01 08:43
No 234488
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

about this: it seems as though the moth balls turn the bromine solution into a gas that then bubbles into the safrole, right??
--------------------
Brominating Safrole

1) Empty your Cl2 gas generator and clean it out.

2) Pop the bromine/catalyst solution into the bottle.

3) Get some old fashioned mothballs. You'll notice that they are nearly 100% naphthalene: perfect, an ideal aromatic. Crush about 100grams of mothballs, not too fine though, leave it chunky. You're going to add this is two additions, so divide it in half.

4) Take the long tube from the gas generator and put it into a bottle of 30gs of COLD safrole. Run the tube through a cold water bath before it reaches the safrole, this will cut down on how much bromine is released (It's not really a prob. but bromine is a volitile liquid). It'd be ideal to have a bromine trap chmaber, but it is optional. The ~30gram bottles of sassfrass work great as a container to brominate in. Plug up the short tube, you're not going to use it.

5) Throw in one half of the crushed mothballs and quickly seal the gas generator. When the reaction stops completely, add the rest of the mothballs and seal again.
 
 
 
 
    AMINATOR
(Hive Bee)
11-08-01 18:04
No 234576
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

I'll answer this question: yes, you're correct just as the post says. Bromine+Napthalene+lewis acid->Hbr(g).
I would chill(-13)the bromine solution and keep it in ice bath during the hbr production.that should help keep the bromine under control. as well as using a drying tube(or small jar filled with crushed damprid/calcium chloride) before the gas hits the safrole which idealy should also be in ice bath for maximum yields.
 
 
 
 
    Bwiti
(Hive Addict)
11-08-01 23:05
No 234644
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

  Why are you folks torturing yourselves trying to produce anhydrous HBr. The DMSO method really works!

  The christian god hates your soul. Care for a little necrophilia?
 
 
 
 
    Agent_Smith
(Hive Bee)
11-09-01 00:06
No 234656
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Nope.  At leats not for me, or the majority of bees.  I suppose it does work in theory, however the DMSO does nothing to prevent cleavage which is the major problem in this area.  In fact as I've said hundreds of times those DMSO color changes indicate everything is going to shit.  Fuck, what do u think is going to happen if you sit safrole with H2SO4 for a few days?!

Granted that everyone gets color changes in DMSO, that means everyone is getting cleavage.  That means that in order to make it work you need to establish a careful balance between the rate of cleavage, and the rate of bromination.  So far no one has given a reliable set of guidelines for temperature, length, ratios etc.  As such, this is still a more robust method, depsite its comparative complexity.

blah blah blah something clever blah blah blah, email at dateline@nbc.com
 
 
 
 
    Bwiti
(Hive Addict)
11-09-01 01:28
No 234718
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

"Fuck, what do u think is going to happen if you sit safrole with H2SO4 for a few days?!"

  Just make sure that you use excess Na-bromide and you won't have to worry. After mixing the bromide/H2SO4, let it sit for 24 hours to make sure all sulfuric acid is neutralized, then add your allylbenzene. Pugsley isn't full of shit.

  The christian god hates your soul. Care for a little necrophilia?
 
 
 
 
    Rhodium
(Chief Bee)
11-09-01 02:06
No 234736
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

The problem is that noone has ever analyzed the composition of the post-reaction "bromosafrole". And I don't think anyone distills it afterwards even, to get an approximate yield determination. According to forensic journals I have in my offline paper archive, the 1-bromo, 3-bromo and 2,3-dibromo compounds are all side products in the reaction, as well as some stuff with a destroyed MD bridge.

Could someone PLEASE distill the formed bromosafrole in any reaction, and then post the yield of stuff coming over at the right temperature (of course after a dilute base wash to remove phenols).
 
 
 
 
    Osmium
(Stoni's sexual toy)
11-09-01 12:48
No 234870
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

I wish I had only half the safrole wasted on this procedure in the last ten years, I probably could fill my big ass party jacuzzi with it.
 
 
 
 
    Bwiti
(Hive Addict)
11-09-01 21:04
No 234925
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

How's this for an idea: Add phthalic or acetic anhydride to a solution of acetic acid, 48% hydrobromic acid, and safrole?

  The christian god hates your soul. Care for a little necrophilia?
 
 
 
 
    Rhodium
(Chief Bee)
11-09-01 22:05
No 234935
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

That would be an idea. Please tell us how it works out.
 
 
 
 
    Bwiti
(Hive Addict)
11-09-01 22:20
No 234936
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

  Could the bromosafrole? be tested by dropping it into cold H2SO4, and hoping it don't dissolve, or is there some other reliable method. Btw, it can't involve distillation, because my vac-pump was cooked by formic acid.
  There is a very reliable way to produce anhydrous HBr, but it might not be for everyone, because I'm guessing that lithium bromide's expensive? Anyway, here's a piece of a patent that gave me a chubby:

US3199953
Process For Production Of Anhydrous Hydrogen Bromide From Lithium Bromide

  Into a turbomixer having approximately a 100ml capacity was charged 61g benzoic acid and 15g (approximately 0.15M) of lithium bromide. The mixture was heated to a temperature in the range 250-260*C with stirring, and nitrogen or carbon dioxide gas at a flow rate of 235ml per minute was passed through the heated mixture. After 1 hour at temperature, approximately 80% of the theoretical amount of hydrogen bromide had been evolved. At 2 hours, 89% of the theoretical hydrogen bromide had been evolved. The reaction is substantially complete after 4 hours of reaction time.
-------------------------------------------------
  In this reaction, would the lithium bromide be converted to lithium benzoate? How would one go about extracting and re-forming the bromide? Peace!cool

  The christian god hates your soul. Care for a little necrophilia?
 
 
 
 
    Bozakium
(Hive Bee)
11-10-01 08:26
No 235111
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

In the lab Br2 is ususlly made by heating NaBr with MnO2 and sulfuric acid.
 
 
 
 
    Bozakium
(Hive Bee)
11-10-01 08:43
No 235117
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

I guess the red P stands in the way of the simple lab prep of HBr from dripping bromine on  RP and H2O mixed with a little sand to slow the rxn. A u-tube with RP dries the gas and removes residual Br2.
  As much as I love industrial chem, I got bromine on me once, and to this day hate the stuff.
  The comment on not being a chem mjr, till p-chem was right, that's a hard fuckin course, and I used to be a physics major, though I came to love both HOMO and his retarded cousin, LUMO.
 
 
 
 
    Gen_Washington
(Hive Bee)
11-13-01 23:13
No 236364
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

I doesnt seem to have been brought since my last post - KBr is no longer OTC in my area - 2 Home Depots that had it dont no more, all replaced (not simply out of season) with much more complicated sounded chems!

Also - could someone estimate amount of Br2 produced by 1 lb of 98% KBr? Is that enopugh for 50 ml Br2?
 
 
 
 
    Karl
(Hive Bee)
11-13-01 23:24
No 236368
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

you should theoretically obtain about 223ml Br2 (density ~3g/ml)
per kilo of KBr
 
 
 
 
    sunlight
(Pioneer Researcher)
11-14-01 00:02
No 236385
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Karl, 223*3 = 669 gr > 1 pound. Check your maths.
 
 
 
 
    Karl
(Hive Bee)
11-14-01 00:16
No 236399
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

SI units are cool
 
 
 
 
    AMINATOR
(Hive Bee)
11-15-01 07:02
No 236911
      Re: OTC MDMA is now easy and cheap!!  Bookmark   

Just to specify the name of the quat sufactant named early, early on in the post. It is Arquad-C50
(n-Alkyltrimethylammonium chloride) from bounce drier sheets.
 
 
 
 
    Peaktime
(Stranger)
01-26-03 22:47
No 401685
      ammonium sulphate OTC  Bookmark   

hello, i'm new around here, I'm from Brazil. I really apreciated your work to turn an completely OTC MDMA synth true.
I've read somewhere around this topic, that there is an easy way of making ammonium sulphate from the Home diluted Ammonia that can be bought in any pharmacy, and would turn this synth more OTC...COuld anybody here tell me this way??
And one more thing... Where should I look for NaBr????And what is his OTC use....
Thanx!!!!!!
 
 
 
 
    hCiLdOdUeDn
(Hive Addict)
01-26-03 23:13
No 401689
      Reacting ammonia with an acid makes an ...  Bookmark   

Reacting ammonia with an acid makes an ammonium salt. E.G.
React NH3 + H2SO4 --> ammonium sulfate

I just read through this thread and I dont understand how it could work. First he starts off with sassasfras oil and doesnt distill anything? And he gets 30% yields from sassasfras, thats crazy. I myself dont believe this procedure.

Sink or SWIM
 
 
 
 
    SpicyBrown
(Hive Bee)
01-26-03 23:17
No 401691
      Well, first off this is a question to be asked  Bookmark   

Well, first off this is a question to be asked in the Chemcals & Equipment forum.

there is an easy way of making ammonium sulphate from the Home diluted Ammonia that can be bought in any pharmacy, and would turn this synth more OTC



Well you could probably get an OTC drain clearing agent that contains sulfuric acid (NOT sodium hydroxide) and neutralize it with fragrance/color-free ammonia. There you have aqueous ammonium sulfate, if you evaporate the water you will have solid ammonium sulfate, the purity of which may be questionable for use in a sensitive synthesis.


Where should I look for NaBr????And what is his OTC use....



You may be able to look at photography supply places.. Its exact use however, will take some research.

-SpicyBrown

--Ahh! Hidden Cloud, you beat me to it. smile

 
 
 
 
    gamilaraay
(Stranger)
03-07-03 05:15
No 414482
      ithink you can obtain ammonium sulphate from...  Bookmark   



ithink you can obtain ammonium sulphate from garden products sulphate of ammonia
here in oz this is what swim uses to make nh3
 
 
 
 
    madprosr
(Hive Bee)
03-07-03 08:01
No 414507
      i saw a pool product consisting of 99% NaBr at  Bookmark   

i saw a pool product consisting of 99% NaBr at a big building supplies store.
it disappeared when the weather got cold, but i'm sure a more specialized store carries it year round.