MDMA synthesis from piperonylmethylketone (PMK/MDP2P) with formic acid

[Montecristo]

how do you use gassed IPA in this situation? How do you know when the ipa has been gassed enough?

 

[Gale]

I gas until I feel its ready, still dialing that. You should bring PH to 5 I believe and then freeze for a few hours.

IPA/HCL will give u same results as gassing at the end if the day, should wash with acetone afterwards anyway.

 

[Gale]

You can weigh the IPA that is a great way to know the concentration. Weigh before and after gassing until lots of gas is escaping and not absorbing into solution.

 

[Montecristo]

so in all the above methods, HCL source should be added till pH 5?

 

[Montecristo]

Okay thank you. what would be a good concentration?

 

[Gale]

I can't recall the exact amount but might as well gas as much as you can or until lots of gas is eacaping and no longer absorbing into IPA. I think you want to aim for 20-30% by weight in HCl.

 

[Montecristo]

okay sweet, sounds the same as concentrating HCL acid.
Thanks for the help.

 

[Montecristo]

If both methods work the same , wouldnt it save a fair a bit of time just using concentrated hcl and IPA?

 

[blackchip]

After the crude mdma is extracted into the diethyl ether, do you vacuum distill off the ether?

 

[WillD]

The product can crystallize in chilled ether

 

[Montecristo]

Any safety concerns on the use of this method?

 

[WillD]

Caution with hot liquids and pairs of formamide and hydrochloric acid. In general, there is no problem, classic Leuckart reaction.

 

[PepitoPistol]

Can any other solvent be used for the extraction?
What's the expected yield of the method?
Dissolving in boiling methanol and quenching in cold acetone doesnt seem very practical from my perspective, because acetone is strictly regulated here. Could it be dissolved in IPA/HCl and cristallized in the freezer? Does it affect yields much?
Thanks!

 

[Gus_Fring]

I know this Method but..is not very good to be true? i mean... whats the trick? low yields maybe? i will try FOR SURE anyway

 

[Montecristo]

Would this method scale up safely? eg 10x or 20x?

 

[RustyShackleford]

Is that because the solvent will take place in the reaction and using DMF would produce MD-dimethyl-A? Both DMF and NMF are difficult to obtain directly for me, and from a quick glance at the preperation of formamide, it looks like I would need methylamine (or dimethylamine) to make them, at which point I feel like it's more practical to just create the imine and gas it with H2, so if I were to do this, I would want to choose an easier to obtain solvent.

 

[Montecristo]

What concentration of formic acid is used? anhydrous? or is 80-85% okay?

 

[Bimbone]

I really hope that this technique will make it possible to make worthy crystals, or at least similar

 

[Fring]

thats a good question... hope the publisher help us.

 

[WillD]

This is one of the classic routes, everything works
Anhydrous formic acid u are unlikely to find. The reaction can be carried out without it, only with N-MethylFormamide