recrystallization of mdma

dr.crack · Thu Mar 03, 2005 3:52 am

Wus just wondering why a lot of the chemistry synthesises talk about recrystallizing the product but no one has said how to recrystallize the final mdma product. Looked all over and finally found something. Can anyone add to this.

It is now time to recrystallize your immensely valuable product. Dissolve
the cake in the minimum quantity of hot methanol. Cool the methanol
solution in the fridge. Crystallization may begin. Layer the solution on
top with an equal quantity of anhydrous methyl ethyl ketone and put beaker into freezer overnight. Overnight the ketone layer will be seen to diffuse into the methanol and a massive crystallization has occurred. Stir if necessary. Some crystals will be needles upto one mm in length. You are laughing. Separate solvent from filter mass using a buchner filter and vacuum. Air dry for a while and then remove residual using a vacuum desiccator. You have a world class crystalline product. You have money in the bank.
thanks.

IndoleAmine · Dreamreader Deluxe

This is one method do do it.

Another one would be to place the dirty mdma in a erlenmayer situated in an oil bath, cover with 60ml MEK per 10g, heat it gently until it starts to boil slightly, and wait for the mdma to dissolve. If it just dissolves partly (most likely), you have to add methanol dropwise with good stirring, until all mdma dissolves. Some small pieces won't dissolve; these are crap and must be filtered. So you vacuum filter the MEK/MeOH/product solution while hot, and return it to the erlenmayer.
Now you continue to heat gently, until the clear solution starts to become slightly milky, then you place a wathc glass on top to prevent the solvent from evaporating, and let it cool very slowly together with the oil bath. At first, nothing will happen, maybe for hours. Continue anyway!
When it has reached room temp., you place it into the fridge (7°C) until it is cool, then in the freezer (-14°C) until it is ice-cold. You have to take care that you don't swirl the solution while transferring the erlenmayer/oil bath into the fridge/freezer, it should stay as undisturbed as possible.
Wait for 24 hours.

At some point between cooling, chilling and freezing, crystals will start to grow, and will continue growing for 24 hours sometimes(!); so you mustn't take it out of the freezer as soon as any crystals appear"

This is the hardest part, you have to wait and wait...
24h is best, 12h is ok too if youre in a hurry.

Then stir the crystals up with a glass rod, vacuum filter while still cold, and wash with a little ice-cold anhydrous acetone, then with some ether if you like, spread out on a glass plate to dry.

i_a

Dr. Weird · Thu Mar 17, 2005 8:16 am

would this way work or do more steps have to be added. The method on this video does not have the fridge or freezer part.
http://www.chem.cuhk.edu.hk/labtech/Videoclip250/RECRYSTALLIZATION.wvx

wolframine · Tue Jun 07, 2005 12:33 am

Nice big crystalls can be formed from a saturated solution of your product in sligtly hot EtOAc/MeOH and acetonitrile. Let the solvent evaporate slowly in the fridge at -4 C or in roomtemperature, this depends on how big you want the xtals Wink