The Vespiary

The Hive => Methods Discourse => Topic started by: silenziox on March 28, 2003, 03:12:00 PM

Title: MDMA & MDA mixture in one rxn
Post by: silenziox on March 28, 2003, 03:12:00 PM: 1. Could mdp2p be aminated to yield both MDA and MDMA
   on one run? I was thinking of the Leuckart rxn, where
   either the ammonium formate/methylammonium formate is
   substituted with mixture of both to achieve the
   favorable ratio for swim.

2. SWIM was wondering after one-night-searching-w/TFSE and
   if there is any method for converting piperonal to
   mdp2p without the nitropropene-step.. With a good
   yield of course ;)

(Btw, Rhodium, the document at
https://www.thevespiary.org/rhodium/Rhodium/pdf/isosafrole.electrooxidation.pdf (https://www.thevespiary.org/rhodium/Rhodium/pdf/isosafrole.electrooxidation.pdf)
doesn't exist...)
Title: That is because I have that article in HTML...
Post by: Rhodium on March 28, 2003, 06:59:00 PM: That is because I have that article in HTML format at
https://www.thevespiary.org/rhodium/Rhodium/chemistry/isosafrole.electro.html (https://www.thevespiary.org/rhodium/Rhodium/chemistry/isosafrole.electro.html)
now.

Barium has posted nice preparations of phenylacetones from benzaldehydes using the Darzen Condensation.

It is always a bad idea to try to produce a mixture of products at the same time. How are you going to purify it? It is hard enough to do even with only a single product.
Title: Hard work
Post by: silenziox on March 29, 2003, 09:02:00 AM: It is always a bad idea to try to produce a mixture of products at the same time. How are you going to purify it? It is hard enough to do even with only a single product.

Thanks for the link of the html-article :)
Why is it that all bees buzz that Leuckart synth is
hard-to-do-synth? I found it to be the easiest synth
(with best yields, thanks to Zealot's improvement!) to
make mda/mdma..

Or did you mean it's hard to purify even single product
at a time? ... How hard could it be if washed with acetone
in buchner?
Title: How hard could it be if washed with acetone in
Post by: raffike on March 29, 2003, 01:37:00 PM: How hard could it be if washed with acetone
in buchner?

Well,acetone shouldn't be considered some wonder cure-all.N-methylformamide gives lower yield than formamide so you probably don't know how much MDA or MDMA it contains without analysis.
Title: Leuckart impurities
Post by: Rhodium on March 29, 2003, 06:58:00 PM: Here below is a review of impurities specific to the Leuckart reaction in the synthesis of amphetamine and methamphetamine. One could very likely assume that similar impurities are present in MDMA and MDA prepared by the same reaction.

http://www.undcp.org/odccp/bulletin/bulletin_1984-01-01_1_page006.html (http://www.undcp.org/odccp/bulletin/bulletin_1984-01-01_1_page006.html)

I think it is extremely naive to assume that all those could be removed by a simple acetone wash. You need to distill the freebase and recrystallize the final hydrochloride to remove the majority of them. And the efficiency of both these purification protocols will be inhibited by using a mixture of MDA and MDMA...
Title: gassing mixture of freebases?
Post by: madprosr on March 29, 2003, 08:25:00 PM: if one gasses a mixture of mda/mdma freebase in toluene, would they get a more homogenous mixture of the two amine salts than if the salts were dried first then ground together?
Title: The mixture would be LESS homogenous if gassed
Post by: Rhodium on March 30, 2003, 12:06:00 AM: The mixture would be LESS homogenous if gassed together than if mixed as powders and sieved through a mesh.
Title: I'm not exactly sure if this is true
Post by: SPISSHAK on March 30, 2003, 10:15:00 PM: You can ask Sam ( I think he mentioned this too) but I think the leukart synthesis when applied to methylenedioxyphenylacetone is more likely to give pyrimidines than the unsubstitued counterpart, as a result isn't an optimal way to produce substitued methamphetamines like this. BTW Rhodium that is an excellent article that belongs on your page.