Chinaman (Stranger)
04-06-01 00:12
No 182458
      safrole+bomb?happy chinaman  Bookmark   

Im having a little debate in my head
could one go about throwing safrole and CH3NH2 into a bomb
to yield mdma without first converting safrole into bromosafrole or mdphenacetone?
greatly appriciate any input into my delema




Remember its illegal we have to get rid of it... puff puff puff
 
 
 
 
    psychokitty
(Hive Bee)
04-06-01 00:23
No 182461
      Re: safrole+bomb?happy chinaman  Bookmark   

No. 

Not yet, at least.

--PK
 
 
 
 
    PolytheneSam
(Master Searcher)
04-06-01 03:05
No 182501
      Re: safrole+bomb?happy chinaman  Bookmark   

Some one I know tried it with 40% methylamine solution, sassafras oil (without purification), a drop of sulfuric acid as catalyst and some transition metal salts as catalyst based on US patent 4937383.  This patent only gives examples of reactions using isobutene, but it looks like it follows Markonikoff's law where if you add R-H across a double bond, the R group goes to the carbon with the least hydrogen atoms.  He tried smoking the residue after the reaction and then later he tried it orally after letting it air out for a while and he found it to be psychoactive.  He saw the brightest colors he ever saw, experienced euphoria and an MDA like high which he was familiar with before.  So if that test was good enough I would say that yes it will work.  I don't know what the yields are.  The sassafras oil was at least 25 years old but still had a very strong safrole smell to it.
You can look up US patent 4937383 using this web page:
http://www.geocities.com/dritte123/PSPF.html


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    Chinaman
(Stranger)
04-06-01 12:54
No 182574
      Re: safrole+bomb?happy chinaman  Bookmark   

Thanks man yea i was thinking about Markonikoff's law that the radical would attach to the most stable carbon
and the secondary C group looks to be the most stable
Thanks again ill have to follow up on the link and do some more research


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    foxy2
(Hive Addict)
04-06-01 20:58
No 182603
      Re: safrole+bomb?happy chinaman  Bookmark   

Sams the MAN
Sams the MAN
Sams the MAN
Sams the MAN
Sams the MAN
Sams the MAN

Thanks for all the kick ass patent work Sam!!!



Do Your Part To Win The War
 
 
 
 
    PolytheneSam
(Master Searcher)
04-07-01 19:17
No 182689
      Re: safrole+bomb?happy chinaman  Bookmark   

I think Chem_Guy was the first one to post things about direct amination.  He listed one or two patents in his thread.  Here's a list of patents on direct amination of alkenes.

2397705 2501509 2501556 2518528 2627526 2984687 4454321 4827031 4929758 4937383 5107027 5900508



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    jim
(Hive Bee)
04-07-01 23:48
No 182755
      Re: safrole+bomb?happy chinaman  Bookmark   

Funny, I tryed posting in this thread yesterday, but I guess it never went thru....  ?

I thought that the high temperatures of this patent would cause isomerization of the allylbenzene double bond forming a propylbenzene. 

The patent does seem to put the amination with a Markinokov addition (nulcleophile to the most substituted carbon).  Which means that the amination works for only allylbenzenes like safrole (if at all).

If you want I can dregde up my old articles and threads, but I think it is all on my website ( http://chemguy.homestead.com )
 
 
 
 
    PolytheneSam
(Master Searcher)
04-08-01 01:09
No 182775
      Re: safrole+bomb?happy chinaman  Bookmark   

Yeah, I never thought about isomerization.  I thought it needed stronger bases like KOH and CaO.  Ammonia and methylamine aren't as strong. The bomb process also seems to produce tar, too, (I don't know if the amine is a solid or not) so it looks like you have some competing reactions.  Maybe this type of process is good if you already have a bomb or autoclave and just want to do some quick experiments with various essential oils.


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    jim
(Hive Bee)
04-12-01 22:19
No 183698
      Re: safrole+bomb?happy chinaman  Bookmark   

I have begun to look at the patents again.  Patents 4,937,383 and 4,827,031 look good.

HOWEVER, I still am wary about the isomerization, but they look easy to test.  # 4,827,031 doesn't look as promising, the pressures are higher, it quotes use for compounds 2-8 carbons long, and uses slightly higher temperatures.

# 4,937,383 looks more promising.  The pressures seem attainable.  The yields are well below 50% though.

US Patents # 5,107,027 and # 5,900,508 seem not too good.  The zeolites, if you can get them, are pretty acidic and might cause ether cleavage and will cause some polyermization.  The patents do state however that they can aminate compounds 2-10 carbons long, even with aryl groups.  The patent DO NOT tell you weather the addition id Markinokovian though, which is of great importance.  If anyone can figure that out please post it...
 
 
 
 
    thunker
(Stranger)
04-24-01 02:09
No 186323
      Re: safrole+bomb?happy chinaman  Bookmark   

How about this untested variation on your idea.  I don't know if this is original or not -- I've never found it in the literature.  If it doesn't work, I'd appreciate knowing the reason why.  If it does work ... crazy
 
 
 
 
    foxy2
(Hive Addict)
04-24-01 05:42
No 186387
      Re: safrole+bomb?happy chinaman  Bookmark   

That is an awsome idea, add a touch of acetone~1ml to aid in the decarboxylation maybe.  And some ammonium sulphate catalyst.

Those pipe bombs scare the shit outta Foxy too though shocked

Someone needs to try this.
You could potentially take undistilled sassy and make E with NO glassware and very little apparatus
smile


Do Your Part To Win The War
 
 
 
 
    Day_Trippah
(Stranger)
04-26-01 06:45
No 186940
      Re: safrole+bomb?happy chinaman  Bookmark   

LOL i like the part about the terrified chemist. I have to say though that this is the coolest shit i have ever read. if this works and it looks like it can, the DEA just got buttfucked. laugh so how 'bout it chemists? by the way i read somewhere that sassy is illegal now? is that true?


coolcoolcoolcoolcoolcoolcoolcool
 
 
 
 
    PolytheneSam
(Hive Addict)
04-27-01 15:31
No 187303
      Re: safrole+bomb?happy chinaman  Bookmark   

The temperature is what drives the reaction not the pressure.  The reason for the bomb is to contain the water and ammonia (or amine) because it would evaporate without it.  OK, if you start with 20 g of CO2 as dry ice in your modification, thunker, what would the pressure be in a 250ml bomb when it turns to a gas at 32-49?  Use the ideal gas equation, PV=nRT.  Also, if you want you can try Van der Waal's equation, too.


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    foxy2
(Hive Addict)
04-27-01 17:37
No 187323
      Re: safrole bomb?happy chinaman  Bookmark   

Yea Sam has a point.  It would bee best to use a high boiling inert solvent for the bomb instead of CO2

Hmmm
para-Dichlorobenzene?
Insoluable in water, otc, easy to wash away with dcm in A/B extraction, boils at 173.4C, melts at 56C.  Heat to 190C or so and away we go.  Pressure probably wouldn't bee an issue becasue the para should stay liquid up to 200C under minimal pressure.  This idea is COOL!!!



Do Your Part To Win The War
 
 
 
 
    jim
(Hive Bee)
04-27-01 19:04
No 187342
      Re: safrole bomb?happy chinaman  Bookmark   

Halide replacement by the amine would be a problem with para-dichlorobenzene...

The pressure in the "bomb" with raise the boiling point of the solvent.  The CO2 could in a a liquid form (supercritical actually) at these high temperaures if the pressure was great enough. 

I have grave reservations about using clandestine chemistry bombs, I would fear for my life.  I would also put at least 2  pressure saftey blow-off valve and a pressure release valve to release pressure when taking off the lid. 
 
 
 
 
    PolytheneSam
(Hive Addict)
04-27-01 19:26
No 187345
      Re: safrole bomb?happy chinaman  Bookmark   

The vapor pressure of water at 250 C is 27 atm.  In P. Chem. lab we were filling bomb calorimeters with 25 atm of O2 before igniting the samples.


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    Day_Trippah
(Stranger)
04-28-01 08:19
No 187508
      Re: safrole bomb?happy chinaman  Bookmark   

So are you saying the bomb would blow?


coolcoolcoolcoolcoolcoolcoolcool
 
 
 
 
    foxy2
(Hive Addict)
04-28-01 10:26
No 187548
      Re: safrole bomb?happy chinaman  Bookmark   

sam those bombs in pchem lab are fucking thick and heavy duty!!!!


Do Your Part To Win The War
 
 
 
 
    PolytheneSam
(Master Searcher)
04-29-01 00:11
No 187679
      Re: safrole bomb?happy chinaman  Bookmark   


So are you saying the bomb would blow?



No.



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    Day_Trippah
(Stranger)
04-29-01 05:06
No 187753
      Re: safrole bomb?happy chinaman  Bookmark   

oh


coolcoolcoolcoolcoolcoolcoolcool
 
 
 
 
    Day_Trippah
(Stranger)
04-30-01 01:54
No 187967
      Re: safrole bomb?happy chinaman  Bookmark   

SWIM will try it if someone would tell SWIM what the fuck glycine is and where/if SWIM can buy it and also the current statis on sassafrass oil legal/illegal


coolcoolcoolcoolcoolcoolcoolcool
 
 
 
 
    Chinaman
(Stranger)
05-08-01 05:08
No 192595
      Re: safrole bomb?happy chinaman  Bookmark   

you can still get sassy oil on the net
but i hear it went illegal
probly just surplus, cant buy more just get rid
of what ya got kinda deal
but im sure you can still get small quantities of it as
aromatic items



My cat keeps talking to me. Should i answer or or finish eating this piece of paper?
 
 
 
 
    PolytheneSam
(Master Searcher)
07-11-01 00:23
No 189903
      Re: safrole bomb?happy chinaman  Bookmark   

I found a patent (US 2449644) on direct amination of stryrenes, propenylbenzenes, etc. using an amine and sodium.  Note the structure in column 2 of the patent:

Ar-CR=CH-R'

If Ar was 3,4-methylenedioxyphenyl, R was H and R' was methyl you should get MDMA.  Here's a new page I made http://www.geocities.com/dritte123/Miscpat.html which includes patents on direct amination.  Note, also, the patents on Wacker/peracid reactions.


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    PolytheneSam
(Master Searcher)
08-14-01 00:50
No 204300
      Re: safrole bomb?happy chinaman  Bookmark   

Here's another interesting direct amination patent.  US 3889600 1-(2-(Phenyl-lower-alkyl)- Aziridines Munition Payload
Not quite an LSD bomb, but almost an ecstacy bomb (uses a related chemical).
Ethylenimine and Na are reacted with a styrene or propenylbenzene to get an aziridine form of a phenethylamine or phenylisopropylamine.  Maybe methylamine will work in place of ethylenimine or maybe methylbenzylamine then hydrogenation.

http://www.geocities.com/dritte123/PSPF.html
 
 
 
 
    PolytheneSam
(Master Searcher)
08-14-01 01:33
No 204314
      Re: safrole bomb?happy chinaman  Bookmark   

These two patents are on amination of P2Ps with alpha-methylbenzylamine which is hydrogenated to get asymmetric amphetamines.
4000197
5360724

http://www.geocities.com/dritte123/PSPF.html


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    PolytheneSam
(Master Searcher)
08-31-01 00:47
No 208787
      Re: safrole bomb?happy chinaman  Bookmark   

The US patent number for the Parr bomb calorimeter is 2065870 .  Its shows detailed plans including cross sections of the parts.  The patent says calorimeter type bombs have to withstand pressures of 1000-4000 lbs/in2



http://www.geocities.com/dritte123/PSPF.html