Question Monomethylamine 40% water

[lucas_cash]

Oke normally I am making mdma with the following chemicals
Pmk oil
Monomethylamine 99%
Methanol
NaBH4

But now I received Monomethylamine 40% water which is giving me a error on, if the water will be a problem for the making of the freebase mdma. Can someone help me with this.

I was thinking about stirring the pmk oil with Monomethylamine 40% water for 10 minutes. And than leave it to rest untill the pmk oil drops to the bottom of the jerrycan and the mono/water will stay above

Than take the mono/water out and leave the pmk oil so I can add methanol to it and continue to adding NaBH4.
Will this be a good way to remove the water out, Or must I leave everything in it.

Does anyone know if the water will be a problem for the whole process?

 

[Tovenaar]

Water will be a problem for the imine forming.. please use methylamine methanol solution, ethanol is also possible. I can remember some nabh4 synthesis with methylamine water solution a long time ago (the time of “the hive”) but from what i remember they all where low on yield (20-35%) This is all from what i remember from a long time ago.. i never tried it myself, also because i always had an supplier for monomethylamine gas, and later for the already made solution in methanol..

 

[lucas_cash]

I always use the Monomethylamine gas
But this time i got the Monomethylamine mixed with water

So you are saying it is best not to use it?

 

[Tovenaar]

I say: give it a try in small scale and report us the results.
If you can’t…. Don’t use it…

 

[lucas_cash]

I am going to try.. will try my method as well. Just take it out after stirring and than continue with methanol
I have no time to order Monomethylamine gas anymore which sucks.

Will report back with results

 

[Tovenaar]

I was reading in old material i still have, and somebody reported 56% with methylamine aqua solution. So please prove me wrong, i hope it will work with better yield!!. It will make everything so much easier. Just order methylamine hcl and make your own methylamine aqua solution 40%, instead of ordering those 200L barrels.

 

[Tovenaar]

The method i would think of would be:
Mixing your mdp2p with methanol, add your methylamine aqua solution, now add your nabh4 under vigorously stirring,

add some extra water, seperate. Cook off the little bit water and methanol left in your mdma base (eventually distill your base, i never did, but some people do. Add your aceton and crystallize with hcl

 

[lucas_cash]

Yes this is the method i was kinda talking about. But instead of starting off with mdp2p and methanol
I was thinking about starting it off with mdp2p and Mono/water solution first.

separate the mdp2p from the mono/water solution.
Than adding the methanol to the mdp2p
than continue the process the way you described it.

Will start on it soon i will add some pictures and results up in here.

Will try both your and my way. Let's see what will happen and how much yield i get out of it.

 

[Tovenaar]

Why i think the procedure you wrote won’t work: methylamine will dissolve better in water, then in methanol.

 

[Tovenaar]

I found an old procedure with mono/water

Borohydride reduction (NaBH4) was performed as follows: aqueous solution (40%) of methylamine (2 ml) was added to a cold mixture of MDP-2-P (1.51 g) in MeOH (5 ml). The mixture was cooled to -20°C and then NaBH4 (30 mg) was slowly added. After dissolving of the reductive agent, the reaction mixture was left at -20°C for two hours. The addition of NaBH4 was repeated three times, in portions of 30, 30 and 40 mg, and the reaction mixture was left at -20°C for 24 h. Methanol was evaporated, 10% HCl (10 ml) was added to a residue, and the solution was washed with CH2Cl2 (3 ml x 8 ml). The organic solution was extracted with 10% HCl, combined aqueous layers were alkalized with 25% NaOH (~10 ml) and extracted with CH2Cl2 (3 ml x 10 ml). Combined extracts were dried over MgSO4, evaporated, a residue was dissolved in Et2O (18 ml), and dry HCl was passed through the solution. The precipitate of MDMA HCl was filtered off, dried and homogenized before analysis.