mdma freebase and crystalization

CharmingKid

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So I have been trying to get mdma in Al/Hg amalgam method from PMK and methylamine and I am not sure what I did wrong- after 6hours I tried to extract the mdma free base with 25% NaOH solution and I needed to pour 100 ml of it until I noticed a change in the consistency and a layer of yellow liquid ( the first 3 photos from the left). After the extraction with NaOH solution and isopropanol I evaporated the IPA under vacuum and did the acid/base extraction with DCM and I gt some liquid in the right color- brown, but it was more like water, not oil (the 4th photo) but I kept anyway and tried to crystalize it with HCl, acetone and xylene and in the beginning it looked like I am going to get some crystals- but I just got something that looked like brown powder in the end (the 2th photos from the right).
Any ideas where i went wrong?
 

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Acidosis

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First, before continuing, check that the brown product you obtained complies with the characteristics of the product, smell, taste and melting point...if it is mdma hcl and it is not some sodium salt or other salts that can be formed by a failed synthesis. dissolve the residue in boiling methanol and allow the solution to cool, it will surely crystallize hard, in which case proceed with a standard cleanup and follow with a second recrystallization and you will obtain the desired product.
 

Curiousonion

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taste??? What is it supposed to taste like?
As for smell it has that gross mdma smell like root beer.
 

Acidosis

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check that its taste is really bitter and if you can check and compare the melting point, if its taste is bitter and reminds you of the mdma that you have consumed, surely you have dirty mdma hcl, now cleaning it and recrystallizing it should be enough, love the smell apparently it smells like the desired product, therefore its synthesis surely worked. time and practice will give you better results. a greeting.
 

Curiousonion

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Yeah i made some that smelled like that 2 days ago. I can't stand the smell though.
Didn't know it was bitter, can't get myself to taste that stuff lol
 

Chemical Ali

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Have you done this synth before but with Nitromethane instead of directly using Methylamine? SWiM prefers it WAY more with the Nitro. Just curious. Guess it's a matter of opinion really. Might be worth looking into.

Kind regards,
Ali
 
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