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Author Topic: 5-Meo-Dmt Synth and Purification.  (Read 252 times)

Trips

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5-Meo-Dmt Synth and Purification.
« on: September 24, 2010, 06:31:09 PM »
Hey All,
I've been looking over the 5-meo-dmt synthesis proposed by Shulgin (oxalyl chloride, amine, LAH) and noted his use of the Kugelrohr.  Curiosity has me wondering if a short-path vacuum distillation apparatus would do the trick if connected to a Hyvac 2 vacuum pump?  The pump is "capable" of 0.5 millitorr, or was at one point.  I don't know what it can do now. 

Does anyone know the temperature of thermal decomposition for this particular compound?  Will boiling take too long with this route?  Or do you think it would be fine?  Would a cold-finger be a better bet?  Would a cold finger work?

Thanks

Vesp

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Re: 5-Meo-Dmt Synth and Purification.
« Reply #1 on: September 25, 2010, 02:07:33 AM »
Since it is probably a small amount, and the substance will have a semi-high boiling/sublimation point I would probably go with a cold finger or perhaps a liebig condenser set up for reflux -- the crystals will deposit in that, which can than be scraped out.
Not to sure how big of an issue decomposition will be so it is risky I guess - but when it is smoked under much less than ideal conditions, it seems to work according to the internet - so I'd imagine in a very strong vacuum with very little oxygen, etc it would work well. 
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Trips

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Re: 5-Meo-Dmt Synth and Purification.
« Reply #2 on: September 25, 2010, 09:07:04 PM »
Hmmm, I thought about the liebig, but Shulgin works with ~12 grams, and since this isn't a real experiment, I will be imagining how I would set it up if I were to do the same. 12 grams is a jammed liebig and an exploded round-bottom, I would think.  But the short path just looks like it has such a long path lol!

My kingdom for a kugelrohr.

Has anyone rigged up a homemade kugelrohr with any success?

-vanadium-

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Re: 5-Meo-Dmt Synth and Purification.
« Reply #3 on: October 02, 2010, 08:27:54 AM »
I personnally would gas it and recristallise it. No need of distillation appartus. Distillation of very high boiling point product is always messy because product can cristallise in the condenser. gissing is a much better way

Trips

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Re: 5-Meo-Dmt Synth and Purification.
« Reply #4 on: October 21, 2010, 06:15:00 PM »
I think thats the whole point of the ball tube.  It is supposed to recrystallize in the condenser.  But for my project I just said I would use a recrystallization.  It worked fine.  Any idea why Shulgin is so adamant on the re-xtal?

letters

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Re: 5-Meo-Dmt Synth and Purification.
« Reply #5 on: November 14, 2010, 05:40:55 PM »
Quote from: Trips on October 21, 2010, 06:15:00 PM
I think thats the whole point of the ball tube.  It is supposed to recrystallize in the condenser.  But for my project I just said I would use a recrystallization.  It worked fine.  Any idea why Shulgin is so adamant on the re-xtal?
the reason real-life chemists are so "adamant" on re-xtalization is this : real-life chemists want their products to be as pure as possible. the fact that your compound is pure white in color and has no smell does not mean that it is pure!
in anyway, i highly recommend using chromatography to purify high boiling tryptamines. yields are usually quantitative. all that is needed is some correct silica gel, a decent buchner, and time. look into DCVC, it is very suitable for larger batches (.5g and above, i know a colleague that used this same technique to purify around 500g of a synthetic aminoester). DCVC details can be found in the blog called CurlyArrow
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