smokemouth (Member)
04-11-00 23:06
No 107752
      First posted 100% OTC dream (told y'all) - Ezekiel  Bookmark   

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   Author      Topic:   First posted 100% OTC dream (told y'all)

   Ezekiel     [Image] posted 08-29-99 10:16 PM
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               The following is all a dream and never actually happened
               in real life:
               Ezekiel decides to make MDA
               First he takes some sassafras oil and rigs up a simple
               distillation with a fridge vacuum pump. He throws away
               the first stuff. When the distillate looks and smells
               right, he collects 70 g. The leftovers are dark red, the
               distillate is clear and smells like heaven. Oh baby!
               Then he adds 7.5 g MgO and 0.7 g KOH, and heats it to a
               boil for 15 min. At this time is it brown and full of
               white and brown particles. After cooling, he add a bunch
               of water, but the solids do not want to dissolve, and he
               gets the most horrible emulsion on the planet. So he lets
               it sit a while, and decants onto a vacuum filter with
               qualitative paper. Lots of crap goes through and the
               paper gets plugged immediately. Argh! Next time, let it
               sit overnight and filter through cotton I think... He
               washes the iso with water till its pale yellow, and plays
               around with the solids for a while. Anyway he finally
               ends up with 40 g iso. What a mess.
               Then he adds 125 mL DCM and 3.75 g Na2CO3 and starts
               stirring in an ice water bath. Over an hour he drips in
               32 mL 35% H2O2 mixed with 72 mL 65% formic acid. He
               assumed they were both v/v when calculating moles. Was he
               right? Since the formic was a little more dilute than
               normal, and the sirring was poor (the magnet kept jumping
               around) he let it stir for 48 hrs. He then separated the
               layers, both orangy, and distilled the DCM off of the
               organic layer. To the residue he added 380 mL water and
               started stirring. Then he added 40 mL 95% sulfuric acid.
               He didn't premix cuz the heat generated boils away the
               last traces of DCM. He heated the mix to 75 oC for 2 hrs.
               The oil was then a dark red. He extracted with DCM,
               washed with saturated bicarbonate, and distilled. When
               the distillate started to get a bit orangy, he stopped.
               The MDP2P was thick and yellow with the slightest green
               tint. Smelled faintly like pepper and burnt wood, but
               sweeter. He got 20.5 g. That's only 46.5 %, but there are
               a lot of things he could have done more carefully, and
               there was not one reagent grade chemical involved, so not
               bad eh?
               Then he decides to make some formamide. He takes 200 mL
               65 % formic and adds household ammonia to pH 8 (1875 mL)
               and puts this in a huge glass pot. He boils it for HOURS
               until the smell changes from ammoniaish to hellish. There
               was only 80 mL left and there should have been 150.
               Doesn't formamide decompose below its boiling point?
               Shit. Oh well, he says, the next part uses a seven-fold
               excess anyway.
               So Ezekiel takes his 80 mL of thick, yellow (huh?)
               formamide and 20 g MDP2P and adds 10 mL water and 1 mL
               glacial acetic acid. He heats this to 150 oC. After six
               hours there is only 7 mL distillate. Strange. When it
               separates, the oil is dark red. He extracts it with DCM,
               washes with NaCl(aq) and distills off the DCM. Mmmm, red
               Then he tries to mix up 27 g NaOH, 125 mL 99% IPA, and 31
               mL water. This forms tree layers. White IPA on top, then
               undissolved NaOH, then really hot, clear water. Oh well,
               make a slurry he thinks, and adds it to the goo and
               refulxes for 45 min.
               At this point ol' Zeke does what I think a lot of new
               bees do. He realizes that he just made X but it's in a
               flask full of crap and he panics. He has never tried MDA
               before and he really loses his cool and strats to goof up
               a lot. So he adds some water to dilute the base, and
               vacuum distills _most_ off the ethanol. (A bunch bumps
               and goes out through the vac line. Ezekiel cusses
               uncontrollably.) Then he extracts a few times with DCM,
               and washes a few times with water. He's left with a dark
               red DCM solution. What to do? He has had very bad
               experiences with the gas; Logical's sulfate method sounds
               appealing but probably won't work in DCM; Sunlight's
               method also sounds good but the solution is REALLY dark
               red; Strike and Chem Abs. say distill, but Zeke is afraid
               he has such a low yield that he will lose it all to his
               enormous glassware. So this is what he does.
               He adds muriatic acid till the solution is pH 8. This
               boils away a bunch of the DCM. This he extracts with
               water. DCM layer is still dark red, water is cream
               coloured. Oh baby, here's where it gets good! He rigs up
               a double boiler and starts to evaporate the water layer.
               Maybe there's some salt in it you think? He gives it a
               taste. ARGCHHH! WOO HOO! It's not salty. Its the best
               horrible taste in the WORLD, amphetamine! In about and
               hour the pan in full of spaghetti-like crystals, cream
               coloured. He crushed them up and weighs. 9.5 g baby!
               Unless you have done something like this before, you have
               NO idea how good it feels to succeed for the first time
               (by a new method at least). He washed them with sub-zero,
               pre-dried acetone. It turnes oh-so-slightly pink and
               leaves behind a mountain of snow. Lucious. This is about
               a 35 % yield, more than he ever got with Al/Hg. Ezekiel
               is very very happy, even though you are all thinking your
               way is better. Ezekiel knows he can improve his method
               and his technique to over 50 %, which is fine in his
               mind. Sassy's cheap and abundand where he lives.
               Then I suddenly awoke from this dream and thought holy
               shit, Ezekiel, I whish I was really you and this wasn't a
               ficticious dream.
               So what's the point? What's the verdict? Lessons learned?
               1. Never be afraid to try new methods. It's easy to think
               one is the best if it's the only one you've tried.
               2. Piss on reagent grade chemicals.
               3. Yield is not as important as saftey, ease, and
               4. Piss on MDMA.
               5. Don't be afraid of emulsions. Better to shake good,
               wait a while and get all the goodies.
               6. Leuckart RULES!
               7. Next time distill the formamide, do a better cleanup
               of the iso, do more thorough extractions and transfers,
               and be wary of the evil bumping.
               8. Always be patient, careful, never panic, and save
               9. Even if others diss you, try your own ideas.
               10. Beg others to help you even if they know you are an
               idiot and they are tired of answering your stupid
               questions. How about some suggestions now?
               Props out to those who made this all possible: Osmium,
               Rhodium, Elusis, Logical, LaBTop, Sunlight, BrightStar,
               Psychokitty, the list goes on you know who you are.. and
               of course, the queen bee herself who wrote the book that
               made it all possible, Strike.
               Never give up, y'all.

               Ezekiel Out.

   Ezekiel     [Image] posted 08-29-99 11:29 PM
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               Ooops. Sorry guyz. Ole' Zeke seems to have forgotten to
               say where he dreamed of getting all this stuff without
               ever even contacting a dangerous chem shop. So here goes:
               sassy: essential oil shop in Ontario, no questions, no
               names, pick-up ($100 per kilo)
               MgO: health food store, in a bottle labelled Magnesium
               Oxide Powder (cheap)
               KOH: take KOH drain cleaner, boil till it gets thick,
               then put it in the fridge; BANG! a zillion KOH crystals
               NaOH: Gillet's Lye (hardware store)
               filter paper: science store (crazy expensive)
               DCM: distill from paint remover
               sodium carbonate: bake some bicarbonate for an hour and
               weigh the difference to make sure you lost the right mass
               35% H2O2: hydroponics store (cheap)
               65% formic acid: tanning shop or bee supply (cheap)
               95% sulfuric acid: "Professional Plumber's Drain Cleaner"
               at Home Deopt (cheap)
               3% white ammonia: grocery store (cheap)
               glacial acetic: photo store
               NaCl: are you an idiot?
               MgSO4: bake some epsom for an hour (cheap)
               99% IPA: grocery store (cheap)
               glassware, hotplate/stirrer, thermometer: science store,
               surplus store, used labware store (price varies wildly)
               vacuum pump: used fridge compressor (cheap)

               So what do you think? No lies or exaggerations are
               involed (except calling IPA ethanol in the previous post;
               we're celebrating a bit here, okay?).

               Ezekiel Out.

   equarius    [Image] posted 08-29-99 11:48 PM
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               Very nice. Think I'll not try the Leukart also.

               Could Ezekiel please email moi at
               or post yours.

               Nice work Cdn bee

   Osmium      [Image] posted 08-30-99 12:44 PM
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               Congratulations! Well done. There might be a few minor
               mistakes in the practical lab work, but it's the success
               that counts. You got your honey and that's the only thing
               that is important.

   psychokitty [Image] posted 08-30-99 07:48 PM
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               VERY well done. I am impressed beyond description.
               Considering your newfound interest in the Leukart
               reaction, however, you may wish to consider doing
               experiments using a microwave as the heat source as
               detailed in a post long ago. As I remember it, the
               reaction scheme was the same, but everything was
               performed in a microwave with the results being a five
               minute reaction time and a yield in the range of 80-90%
               with no tar formation. Since it appears that sassy will
               be available in your locale for quite some time, you
               could really do the Hive a favor by conducting research
               in this area.

               As for your problems regarding gassing and such, you may
               wish to give my OTC anhydrous HCl gas generator a shot.
               Details of its construction and operation can be found on
               Rhodium's page.

               Good luck to you in the future and keep up the good work.


   psychokitty [Image] posted 08-30-99 09:36 PM
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               Thought that you might find this interesting:

               Taken from JACS Feb. 20, 1953, vol. 75, pp. 921-925.

               (b)Leukart Reaction--To a three-necked, 2-Liter flask,
               fitted with a dropping funnel, a thermometer reaching to
               the bottom, a stirrer and a Friedrich condenser arranged
               for downward distillation was added 315 ml of 28% aqueous
               ammonia. To this stirred solution was added dropwise 264
               ml of 90% formic acid. The stirrer was removed and the
               solution was heated gradually over a 2 to 3 hour period
               to 160 deg C, the temperature being regulated so that
               fairly rapid distillation took place. After cooling to
               110 deg C, 164 g. (1.0 mol) of o-methoxyphenylacetone was
               added and the mixture heated at 160-170 deg C for 5
               hours. At the end of 2 hours the upper layer of the
               distillate was retured to the reaction. After standing
               overnight the homogenous solution was heated 2 hours
               more. It was then cooled to 70 deg C, 360 ml of
               concentrated hydrochloric acid was added dropwise and the
               mixture heated for 6 hours under reflux and allowed to
               stand overnight. The suspension was diluted with 600 ml
               of water and extracted with benzene. The aqueous layer
               was basified, extracted with benzene and the residue from
               the benzene distilled under an atmosphere of nitrogen;
               b.p. 118-122 deg C at 11mm, yield 95 g. (58%).


   Ezekiel     [Image] posted 08-30-99 09:56 PM
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               Thanks PK. Now THAT is the kind of feedback I need. Wow.
               I was assured by someone that the formamide could not be
               generated in situ. Will have to dream.

               Os- what suggestions do you have.
               Please don't tell me to gas. I will next time.

               BTW, biological test dreams were amazing.

               Ezekiel Out.

   Ezekiel     [Image] posted 08-30-99 10:44 PM
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               Sorry, I reread that and it's not really in situ, it's
               just in the same pot before the reaction.
               I talk too much, too fast.

               Searched all microwave articles, none on the Leuckart
               found. I'm really interested now though.

               Ezekiel Out.

   psychokitty [Image] posted 08-31-99 05:30 PM
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               Using the Hive's search engine doesn't always work. Ever
               since the last crash, there has been considerable trouble
               experienced by many bees while attempting to locate
               threads using keywords or phrases.

               Anyway, the thread you are looking for is called "Son of
               Leukart arises to battle the evil Narc hordes" by Cherrie
               Baby. There were ten posts to date with the last one
               being on 12-11-98 at 5:37 a.m. Oh yes, the thread can be
               located under the Novel Discourse section of the Hive.
               You'll have to access all of the topics from the last
               year in order to get to it, but that really shouldn't be
               all that much of a problem.


   daragh      [Image] posted 09-01-99 03:28 AM
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               Nice one ,And i'm just about to do my weekly grocery
               shopping. Me thinks i'll be picking up a few extra otc

   hellman     [Image] posted 09-01-99 08:07 PM
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               Was in the area, so just popped in to say..

               Your're on fire Ezekiel,
               I take my hat off to ya!.
               This is the kind of shit we want to see.
               Fuck Hg salts,
               Although one question still haunts me.

               How do we make n-methyl formamide to go on to mdma?.
               I would like to see that.

               cool man, well done!


   psychokitty [Image] posted 09-01-99 09:26 PM
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               Why not just reduce the N-formyl-MDA that is formed in
               the first part of this reaction catalytically or with a
               hydride to MDMA?


   Ezekiel     [Image] posted 09-01-99 11:00 PM
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               CATALYTICALLY? Got a reference for me?
               No hydrides at Home Depot this week. :-)

               Ezekiel Out.

   psychokitty [Image] posted 09-02-99 06:29 PM
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               Catalytically?: In other words, using Pd/C or Pt/C and
               hydrogen under pressure.


   dpHarma     [Image] posted 09-03-99 12:59 PM
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               fascinating report!

               couple questions.

               1. did you use the 65% acid 'straight' from the jug? was
               it from bee-keeper's?
               (SWINM found when distilling from the jug the first time,
               lots of crud was left behind in the flask)

               2."He adds muriatic acid till the solution is pH 8. This
               boils away a bunch of the DCM. " is pH 8 correct? the
               heat of adding the acid boils the DCM away?
               "this he extract with water"
               so you have a two phase sol'n (DCM/prod and conc. HCl) w/
               the pH of the aqueous layer slighly basic by
               then add water to 'dilute' the aqueous layer and
               is the layer still pH 8? when you boil off the liquid?

               thanks for the inspiration


   Ezekiel     [Image] posted 09-03-99 03:14 PM
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               My mistake. Should be pH 5, which would make a lot more
               sense. And yes, adding muriatic heated the solution
               enough to boil off some DCM.
               Untouched beekeeper's formic was used, but will be
               distilled if Ezekiel dreams again.
               MUCH could be improved. This was just a test.

               And I'm going to have to go back on my word... MDMA is a
               LOT better. All Zeke would need is an OTC HgX source and
               we're off to the races on that one too!

               Ezekiel Out.

   Atomicdog   [Image] posted 09-04-99 11:55 AM
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               Kitty - Could you please expand on how to adapt this
               simple little reaction to produce MDMA? The leukart is so
               easy, this could really ressurect the dreams of an old

   psychokitty [Image] posted 09-05-99 01:51 PM
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               There really is not much to it. N-formyl-MDA is the
               intermediate that is formed from reaction of formamide
               and MD-P2P. If one hydrolyzes this using HCl of NaOH
               solution, one will get MDA. But if one reduces the
               N-formyl-MDA instead using lithium aluminum hydride or
               Pd/C and hydrogen or any of the other newer ways of
               reducing amides, one will get -- as a result of the
               reduction of the carbonyl group on the amide skeleton --
               MDMA. In PIHKAL, I believe that Shulgin synthesizes MDMA
               from MDA by first formylating MDA and then reducing it to
               MDMA. In this case, use of the leukart allows you a
               direct way to the N-formyl-MDA.
               Basically, you would make use of Shulgins second
               reduction step to get your product.

               That was rather long winded. But I'm sure you get the
               picture. And if you don't, I'll be happy to try to
               explain everything again.


   Atomicdog   [Image] posted 09-05-99 04:27 PM
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               Hmmm... it seems to use some chems that would require a
               supply house, and some experimentation(isolating the
               M-formyl MDA, etc...). the other problem is buying
               LiAlH4, is that a watched chem? Probably, so whats the
               best way for a hack like AD to proceed in terms of chems
               needed and rxn touchiness?

               The more i look at this the more i wonder why the leukart
               isn't more popular. It's realatively easy, needs no
               exotic chems, and doesn't screw around with mercury!

               If I did that sort of thing, I'd work this bad boy up and
               start converting the masses.

               lets talk more PK,
               AD out

   hellman     [Image] posted 09-05-99 07:46 PM
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               Atomic Dog,

               I feel the same way,.


               To not make homemade Hg salts, refer to the thread
               called, Hg and it's salts, by Moi!.
               Or just grind together some iodine and mercury from a
               thermometer. Add excess iodine to convert all the Hg,
               then evap the excess iodine off in the dark, in a warm
               place. You will see a fine scarlet sand remain, It's
               beautifull, as far as hg salts can be that is!.
               What's mda like anyway?


               I sometimes wonder about making formamide from formic
               acid and urea, as posted by everyman, one would think
               that you would need a lot of cuso4 to firstly obtain
               close to 100% formic acid.

   Ezekiel     [Image] posted 09-06-99 04:56 PM
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               To add to the long list of opinions, MDA seemed great at
               first, but after a few tries, I'd have to say MDMA is
               MDA's cool cuz it's easier to not make, and after it
               comes on, it's really good for about an hour, like MDMA
               without as much magic, but then it lingers on forever
               with a really amphetamine-edge. Comedown is a LOT
               smoother than MDMA, but I seem to get a bad hangover from
               MDA, none from MDMA. Taking a lot of MDA >150mg gives
               great visuals, but more hangover (for me anyway). I'd say
               a hit of MDMA and then another half-hit an hour into it
               would be my personal favorite. For jaw clenching, I suck
               on DXM lozenges - it may reduce wear and tear on the

               A 100% OTC MDMA synth is about a week or two away,
               because it needs to be not-tested a few times first.

               Thanks everyone for the encouragement.

               Ezekiel Out.

   hellman     [Image] posted 09-09-99 01:20 AM
               [Click Here to See the Profile for hellman]
               Unless I beat you to it,.

               I'll race you for a good n-methyl-formamide synth.



   Atomicdog   [Image] posted 09-09-99 06:25 PM
               [Click Here to See the Profile for Atomicdog]
               Are you sure you made formamide? I read in the 'son of
               leukart' post that Formic acid + ammonia produces
               ammonium formate. I don't have my Merck on hand, so I'm
               talking out my ass, but if ammonium formate is a stable
               solid then that may be even better from a ease of use
               In that same post I read that formic acid + urea does
               produce Formamide, but, if formamide is unstable as you
               said(again, no Merck!) then screw it! Stay with ammonium
               formate, its only 2% to 10% yield diff which is
               negligible if you can get 50% from this.

               I say again, this may prove to be THE method for hacks
               and pros alike if the microwave thing works out. The real
               successor as champ over the Al/Hg. I LOVE no mercury man!

               I'm working up a procedure with scaling from all the refs
               I can find on this, but there really should be a
               formamide/ammonium formate snyth section on Rhods page,
               I'll email him.


   hellman     [Image] posted 09-09-99 10:35 PM
               [Click Here to See the Profile for hellman]
               If you could get 100% formic, say via drying with cuso4,
               The Urea+formic. would be the way to go.

               Does anybody know if water eill fuk with this?

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(Hive Addict)
02-05-02 23:17
No 265621
      Re: First posted 100% OTC dream (told y'all) - Eze  Bookmark   

Yes, he added the distilled safrole to KOH with the magnesium to dry it. Then heated to boil (reflux). That would make isosafrole.

It is cleaner if you omit the magnesium, and use a vacuum while refluxing several hours (6-8).

It looks like he used washes to clean it, but distillation is preferred, under vacuum or not.

Real men cook naked.
(Stoni's sexual toy)
02-05-02 23:23
No 265626
      Re: First posted 100% OTC dream (told y'all) - Eze  Bookmark   

Also, MgO cannot be considered a drying agent. But it should clog your filtration pretty well.

I'm not fat just horizontally disproportionate.
(Hive Addict)
02-06-02 00:32
No 265645
      Re: First posted 100% OTC dream (told y'all) - Eze  Bookmark   

I just want to acknowledge that Ezekiel was one of the old bees that I looked up to at the Hive. Hats off to him, I hope he's doing well! Chromic loves your ingenuity. smile

Anyways, he made a mistake in making his isosafrole. He should have omitted the MgO, maybe he thought it would be a good substitute for CaO, anyways, he should have left it out.

Also he made a mistake in making formamide. He should have used a vigreux column when distilling down the water off from that large volume, then once the liquid gets to about 150C, he should have then concentrated (and perhaps distilled) it using an aspirator vacuum.

HoH, here's a synopsis (in chronological order) of what Ezekiel did so you can follow his post:

1) distilling sassafras to safrole
2) safrole to isosafrole (KOH/MgO--again, do not use MgO!)
3) isosafrole to mdp2p via performic
4) makes foramide via household ammonia and formic acid (vigreux column, distill out all water using vacuum)
5) mdp2p to mda via Leukart
6) MDA to MDA.HCl via an acidic water extraction
(Hive Addict)
02-06-02 05:24
No 265743
      Re: First posted 100% OTC dream (told y'all) - Eze  Bookmark   

The reason he chose that method is because everything was OTC. PdCl2 and benzoquinone were a bit more obscure back when he wrote that... Bright Star hadn't yet posted his dreams re:the wacker...
(Junior Service Representative)
02-08-02 05:03
No 266736
      Re: First posted 100% OTC dream (told y'all) - Eze  Bookmark   

               Or just grind together some iodine and mercury from a
               thermometer. Add excess iodine to convert all the Hg,
               then evap the excess iodine off in the dark, in a warm
               place. You will see a fine scarlet sand remain, It's
               beautifull, as far as hg salts can be that is!.


(Hive Addict)
02-08-02 06:21
No 266760
      Re: First posted 100% OTC dream (told y'all) - Eze  Bookmark   

Distilling sulfuric acid is nearly impossible. I've tried it before... good luck.

65% formic acid can be distilled to remove non-volatiles, and apparently it works well.
(Stoni's sexual toy)
02-08-02 11:20
No 266867
      Re: First posted 100% OTC dream (told y'all) - Eze  Bookmark   

> Can someone please describe the odor.. I have nothing to
> refer pungent to.

It stinks.

> How would you seperate the two via distilliation?

You can't.

> I suppose you wouldn't really have to if water was the
> only other thing in it...


> Wouldn't it burn you if you put it on yourself?? Ahhh!

Yes. Ahhh! As in ouch.

> Maybe give you a fake a tan!!?? Hrmm.. Am I close?

No. This has nothing to do with suntan. It will destroy your skin if left there for a while.

I'm not fat just horizontally disproportionate.
02-08-02 11:22
No 266868
      Re: First posted 100% OTC dream (told y'all) - Eze  Bookmark   

I suppose you wouldn't really have to if water was the only other thing in it... Im just not picturing what it would look like if accuired from a tanning salon..

What... no you silly billy not a tanning salon (Where people get all suntaned)

But it is use in tanning hide/leather... now thats something completly different...

Don't wander into a Tanning (Suntan Shop) and ask for formic acid....they will look at you blankly

I love the smell of Ketone in the morning.