Honestly it's not the best method.
There is another rxn writeup on this thread where they use 180 to start on an industrial scale. They distill the formic acid they don't reflux it and I understand why, too much acid to neutralize at the end.
But now I'm having trouble crystalizing it.
I added...
On second try I refluxed it with the hcl for 6 hours. It stayed a brown liquid.
I added naoh solution to bring ph up (takes a lot of naoh in order to do that).
Seperated with dcm after, separation has a lot of salt residue in it.
Evaporated the dcm and got left with a brown syropy liquid.
I...
No, not yet.
Trying the reaction again today but going at 45-55c for 6 hours instead of higher temp for 3 hours.
So far it looks better than the previous reaction, it did not turn into tar although it was not a clear yellow after the 7 hour reflux with formic acid as described by op.
On the vespiary. Won't let me paste the link on here for some reason.
Also some claims that dcm makes the best mdma crystals and other claims that say it is impossible to crystallize mdma in dcm.
I tried this conversion recently, did the nmf with formic acid and pmk reflux for 7 hours. Cooled it down then added the 37% hcl, no reaction since it is acid to acid.
Then started refluxing it, as soon as it went over 84c the mixture started to turn into a brown sludge.
I think its wiser to...
That method is for methamphetamine synthesis which is sensitive to water.
Since you are making mdma base I don't think the reaction needs to be kept anhydrous so the addition of the dessicant is not necessary.
Any one has any opinions on this?
Once you do the ipa separation you usually vacuum distill the ipa off.
Some people also do a steam distillation of A oil after that to remove every unpleasant smell and make it ultra pure. (but people don't recognize A oil without the stinky smell usually)
I read a lot of conflicting reports about crystallizing mdma from DCM.
Some say it gives the cleanest and best crystals and others say mdma freebase will never crystallize in DCM.
Anyone has any experience and can chime in?
Interesting, I read on a synthesis paper that low temp can lower the yield.
How low would you recommend? Cause if it can go below zero then the addition could be done extra fast