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Suggestions to separate 3,4-methylendioxy-N,N dimethylampetamine from 3,4-Methylenedioxymethamphetamine

indigoaura

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Jan 4, 2009
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I have a sample of MDMA that is contaminated with 3,4-methylendioxy-N,N dimethylampetamine (according to lab results).

I would like to separate the contaminant 3,4-methylendioxy-N,N dimethylampetamine from the 3,4-Methylenedioxymethamphetamine.

The sample was already washed with acetone and re-crystalized, so that did not do it.

Any suggestions on how to separate the two and maintain the integrity of the MDMA?
 
Reflux with nitrous acid (potassium nitrite & hydrochloric acid). Then basify with sodium hydroxide and extract the N,N- dimethyl compound with ether. The aqueous soln should contain the nitrosoamine formed from MDMA. This can then be hydrolysed by refluxing with hydrochloric acid.
This method has one drawback; if you don't hydrolyse ALL of the nitrosoamine, you have yourself enough tip top carcinogen to ruin your life.
All things considered, column chromatography is probably a better bet, even if it is a pain in the arse...
 
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