The final product had a faint smell of MeAm and tasted different. When tested it became clear that there was meam in it.Tested how?
Smell and taste is not an adequate analysis method to differentiate between different amines, as most aliphatic amines have a very similar smell. If you vacuum distilled the MDMA, the MeNH
2 would evaporate. Also, it would have formed MeNH
2.HCl when you crystallized the MDMA.
I believe that you simply did not recrystallize your MDMA.HCl properly, and what you smell/taste are either residual MDMA freebase, alternatively unknown byproducts carried over through the distillation.
Anyhow, whatever the identity of the amine-smelling impurity, it will be removed by recrystallization of your MDMA.HCl. Preferably recrystallize from 7 mL/g boiling acetonitrile, but you can also dissolve the salt in a minimum of boiling isopropanol, and then with good stirring add
just enough acetone (or preferably diethyl ether) to form a lasting turbidity
* in the solution. Stop the stirring, and allow the MDMA.HCl to crystallize at room temp for ~30 minutes, then filter, and wash the crystals with a little acetone (or ether), then place the filtrate in the freezer a couple of hours to recover a second crop (less pure) of MDMA.HCl, but this will amount to much less than the first crop. As this second crop is of lesser purity, you should ideally subject it to another recrystallization, and you
definitely should if it visually looks worse than the first crop.
Note to everyone: This is a perfect example of why it is preferable to both distill your MDMA freebase, as well as recrystallize the MDMA.HCl afterwards to achieve a high purity of your final product. The A/B extraction before the distillation is even more important, but you hopefully already knew that, didn't you? Factoid: Recrystallizing (already purified) MDMA·HCl from boiling THF (~130mL/g) gives an insanely low density microcrystalline powder (unusable as purification method, but for you who want to choose your crystal size...)
*turbidity
(
http://dictionary.reference.com/search?q=turbidity)