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Author Topic: Methylate MDA freebase to MDMA???  (Read 523 times)

German

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Methylate MDA freebase to MDMA???
« on: December 05, 2009, 06:45:24 AM »
First thought of zinc and formaldehyde, then was told zinc and paraformaldehyde would be much better, now being told that might not be a good way to go either. Any ideas?

Sedit

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Re: Methylate MDA freebase to MDMA???
« Reply #1 on: December 05, 2009, 07:14:32 AM »
I dont know but I must ask this as well... This is a reductive amination using MDA as the amine source and Formaldahyde as the aldahyde or ketone to be aminated..... can some one please explain to me why the fuck im still tasting Mercury when I play with my chemicals? It appears Zinc can perform the same exact thing so why oh why fuck with Hg?

I may just have to aminate some acetone to perform some test when I can.
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German

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Re: Methylate MDA freebase to MDMA???
« Reply #2 on: December 05, 2009, 07:28:07 AM »
^^^ Dude I'm pretty sure you aren't suppose to eat Mercury. I think I read that somewhere.

jon

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Re: Methylate MDA freebase to MDMA???
« Reply #3 on: December 05, 2009, 11:36:32 AM »
well here's the scoop that zinc/ formalin system  has been tried it has to  be basic and it's very ph sensitive and touchy and accoriding to anecdotal accounts failed to work.
might i suggest tweaking the clarke esheweiler system's stochiometry and reducing rxn time to favor mono amine formation seems to be hard to fuck up.
does'nt mean the xzinc system would'nt work but it may require expirimentation and exact parameters.
« Last Edit: December 05, 2009, 11:40:32 AM by jon »

no1uno

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Re: Methylate MDA freebase to MDMA???
« Reply #4 on: December 05, 2009, 01:52:57 PM »
Quote from: Sedit on December 05, 2009, 07:14:32 AM
I dont know but I must ask this as well... This is a reductive amination using MDA as the amine source and Formaldahyde as the aldahyde or ketone to be aminated..... can some one please explain to me why the fuck im still tasting Mercury when I play with my chemicals? It appears Zinc can perform the same exact thing so why oh why fuck with Hg?

I may just have to aminate some acetone to perform some test when I can.

Eating mercury - even accidentally handling organomercury salts scares the living shit out of me (for good reason)... Chance discoveries with Hg (eg. that dimethylmercury is not a good thing to handle with latex gloves) tend to involve the death of the person on whom the discovery was made... Eating it, damn I still shudder to think of the amount of the element I've breathed in (I used to scrounge it from old neon light tubes from a closed down nightclub, for no particular purpose at the time - just break the tube and tip the small amount of the element into water - now I'd break it under water - with ice, but not to worry couple of g's of Hg won't hurt in the long term, surely)
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German

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Re: Methylate MDA freebase to MDMA???
« Reply #5 on: December 05, 2009, 06:57:57 PM »
Quote from: jon on December 05, 2009, 11:36:32 AM
well here's the scoop that zinc/ formalin system  has been tried it has to  be basic and it's very ph sensitive and touchy and accoriding to anecdotal accounts failed to work.
might i suggest tweaking the clarke esheweiler system's stochiometry and reducing rxn time to favor mono amine formation seems to be hard to fuck up.
does'nt mean the xzinc system would'nt work but it may require expirimentation and exact parameters.

I already went through a shit show trying to methylate alanine with zinc and formaldehyde and that fiasco was documented over at WD, but I was told methylating MDA should be much easier then alanine.  And it better be because I sure would hate to have to go through as much MDA as I did alanine. Going through kilograms of $60/kg alanine is one thing but going through kilograms of MDA is not something I can stomach so I'd like to get the theory worked out as best as possible before I start throwing tons of MDA down the drain.... Btw, you are right about the pH being the key, at least that is what it seemed when I was trying to do alanine.
« Last Edit: December 05, 2009, 07:55:13 PM by German »

jon

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Re: Methylate MDA freebase to MDMA???
« Reply #6 on: December 05, 2009, 09:05:28 PM »
reducing temperature, adjusting stoichiometry and, possbly other variables could make clarke esheweilier the route of choice think about it.
if i had time i's run that system and spot it in silica plates and find out the parameters but i don't have the time right now i'd crack that nut willl one day.

German

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Re: Methylate MDA freebase to MDMA???
« Reply #7 on: December 05, 2009, 09:08:30 PM »
I think I may just make MDMA from scratch. Below doesn't seem too difficult or use hard to find chems. It may be a much bigger deal then a simple methylation but at least I know it works.

http://www.erowid.org/archive/rhodium/chemistry/brightstar.mdma.html

jon

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Re: Methylate MDA freebase to MDMA???
« Reply #8 on: December 05, 2009, 09:12:54 PM »
talk to the old school x cooks the vcold method, iodosafrole or catalytic hydrogenation is how it's done on a large scale  shit fuck all tha tedium.

heisenberg

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Re: Methylate MDA freebase to MDMA???
« Reply #9 on: December 06, 2009, 01:22:57 AM »
If worst comes to worst, the MDA could be converted to MDP2P. Then any of the standard reductive amination methods would apply.
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German

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Re: Methylate MDA freebase to MDMA???
« Reply #10 on: December 06, 2009, 02:15:24 AM »
Quote from: heisenberg on December 06, 2009, 01:22:57 AM
If worst comes to worst, the MDA could be converted to MDP2P. Then any of the standard reductive amination methods would apply.

Hell that would be fine with me. I mean instead of doing 1 step you are doing 2, big deal. I'm not familiar with turning MDA into MDP2P though. I'm sure a quick search will remedy that.

heisenberg

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Re: Methylate MDA freebase to MDMA???
« Reply #11 on: December 06, 2009, 02:27:59 AM »
Crap, I might have spoken to soon. I assumed it was possible, and probably written up. I'll look more into it.
I spent all my money on booze and hookers, the rest I wasted - Charles Bukowski

jon

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Re: Methylate MDA freebase to MDMA???
« Reply #12 on: December 06, 2009, 03:19:47 AM »
man what about clarke esheweiler?? just adjust the time and stoichoimetry

Enkidu

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Re: Methylate MDA freebase to MDMA???
« Reply #13 on: December 07, 2009, 05:29:18 PM »
Quote from: heisenberg on December 06, 2009, 02:27:59 AM
Crap, I might have spoken to soon. I assumed it was possible, and probably written up. I'll look more into it.

pretty sure (di?)chloroamine hydrolysis will do it.... better double check though

German

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Re: Methylate MDA freebase to MDMA???
« Reply #14 on: December 07, 2009, 05:40:11 PM »
Quote from: jon on December 06, 2009, 03:19:47 AM
man what about clarke esheweiler?? just adjust the time and stoichoimetry

Ding ding ding. And we have a winner. Thanks jon (someone else just sent me the reference). Nothing but paraformaldehyde, oxalic acid, and 1 hour of time for very excellent yields.

java

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Re: Methylate MDA freebase to MDMA???
« Reply #15 on: December 07, 2009, 06:07:45 PM »
Reference Information


A Solvent-Free and Formalin-Free Eschweiler-Clarke Methylation for Amines
Thomas Rosenau,1 Antje Potthast,1 Ju¨ rgen Ro¨ hrling, Andreas Hofinger,1 Herbert Sixta,2 and Paul Kosma
SYNTHETIC COMMUNICATIONS 32(3), 457–465 (2002)


Abstract:
Primary and secondary amines are N-methylated by a mixture of paraformaldehyde and
oxalic acid dihydrate in good to excellent yields. The reaction proceeds without
involvement of organic solvents and toxic formalin. Reaction temperatures of 100 C are
required for the decomposition of oxalic acid into the intermediate formic acid which acts
as the actual reductant. The reaction conditions have been optimized, and the mechanism
has been elucidated by means of deuteration experiments.



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POSEIDON

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Re: Methylate MDA freebase to MDMA???
« Reply #16 on: December 08, 2009, 08:36:59 PM »
Quote from: German on December 05, 2009, 06:45:24 AM
First thought of zinc and formaldehyde, then was told zinc and paraformaldehyde would be much better, now being told that might not be a good way to go either. Any ideas?
Hey look in  the article method II
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jon

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Re: Methylate MDA freebase to MDMA???
« Reply #17 on: December 10, 2009, 04:12:01 AM »
paraformaldehyde = campachem
oxalic acid won't bat an eye either it's a green light G O go
like i said if, i had time i'd run it and report back, but i dont'
speaking of which this would be a damn good method for making dmt from trpytamine jon wonders if acetaldehyde would work just the same or is this a special case?
if not the orally active Diethyltryptamine could be easily had too by substituting acetaldehyde;
a good lsd substitute.
would someone more knowledgeable than myself care to elaborate???

p.s.

campachem contains dyes and surfacants that tend to foam the fellas at SM suggest to wash this out with alcohols however, expiriments have prooven that water works the best.
« Last Edit: December 10, 2009, 04:32:31 AM by jon »

shroomedalice

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Re: Methylate MDA freebase to MDMA???
« Reply #18 on: December 11, 2009, 06:41:10 AM »
thats one that slipped me by det nice ill look into that. I didont know all you needed to do was change the amine
too diethyl to get activaty oraly :)

Carrion Fairy

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Re: Methylate MDA freebase to MDMA???
« Reply #19 on: December 11, 2009, 07:15:49 AM »
I don't know about methylating phenethylamines but it will not work to methylate tryptamines, a pictet-spengler reaction will occur instead, forming a ring structure.
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