Mephedrone (4-MMC) Synthesis [2B4M, Ethyl Acetate, Methylamine HCl]

[Dr. MMX]

I used more amount of solvent to make more quick reaction and to not get such such big temperature, it can be used with different proportions but I think minimum is 350-400 ml.

The method was only in the case when the aq40% is not aviable or for some reason it not result good synthesis. Method is not scalable very much, it will rinse a lot of problems when scaled up but its ok for this scale.

If somebody recieve smaller yield there can be a lot of reasons, based on the purity of regents used, the techniques performed.

The 2i4m probably could be used but I did not test it.

If you do have bad yield or your reactoin turns out not clean - please do remember that using methylamine hcl rather than aq results more impurities, as well the alcohol with metylamine. The reaction must be performed ASAP with no futher delays until acidificatoin. Longer it takes worse result will be.

Regards.

 

[Alchemistfromthahood]

I replaced the aqueous solution with hydrochloride because the smell is unbearable and everything smells of this chemical. Why do you think the synthesis isn't scalable? I've processed up to 5 kg of the precursor using your method and always had a yield between 55-60%. Aside from the fact that you do a bit of extra filtering, this route is very convenient in terms of handling.

 

[Alchemistfromthahood]

What I've noticed is that the longer the free base is left unacidified, the darker the color becomes. The free base starts off a beautiful yellow with a certain color density, then changes to green or dark green. However, this problem can be easily managed with a few optimizations in the workflow.

 

[Dr. MMX]

@Alchemistfromthahood
there is high chances that the product was not 4mmc in the most, just some solid masses.
Alcohols do react with methylamine and its basicly methylamonium released instead of methylamine.

For the fast and otpimal synthesis the best is dcm and dmso/nmp/dmf.

 

[Alchemistfromthahood]

You mean combining two solvents? Sounds interesting, and you say it's the optimal synthesis route for mephedrone. I'll try it out soon, and thanks for the tip.

 

[Russian lab assistant]

Together?

 

[Alchemistfromthahood]

@Dr. MMX
i think I would try this way
do you have written down a synthesis route or something similar ? thx for your time

 

[achemica2500]

what changes in the procedure in case of change solvent (dcm or dmso) ?

 

[Russian lab assistant]

You need to monitor the temperature. So that the temperature does not exceed 35-37C’. DCM starts to boil at 39.8-40C’.

try to keep a bath of water and ice nearby. At 35C, immediately transfer the solution to a cold bath and stir. (don't forget to wear a mask!)

The main thing is to add NaOH in parts, the first half in a thin stream and put methylamine hydrochloride, repeat this several times, watch the temperature!!! If your solution turns blue, don't worry, just stir more intensively. or you can already separate!

DCM is great for beginners, you can take a small flask (so that both hands can grasp it), and conduct tests on it. Thus, when you touch the flask with two hands in gloves... you get used to it and understand what temperature is in the flask now.

Good luck with the synthesis! Remember: the lower the temperature, the longer the synthesis, the lower the yield. Everything comes with experience. Experiment, my friends!

 

[Dr. MMX]

There is no alternative to change in this particular case, I do tihnk that its not optimal to use DCM becase the reaction is too long, while we do use methylamine HCL which leads to more impurities, however reaction has its pro that it can be even done as " 1st job".

DCM preferably with other solvents preferably dmso or nmp is reaction that rarely exceeds 40 mins.
The precise dosage of methylamine aq is the key, combined with speed of stirring we can control exhotermic reaction. I suggest to start from 20g of 2b4m, 45-55 m of dcm at 20c and 12-16 ml of dmso/nmp. Nmp is added to DCM, then 2b4m is dissolved.
Recommended equipment is mechanical stirrer with precise regulatoin of the stirring, three necked flask, thermometer probe (glass).
We can add methylamine all at once (35ml), but using the funnel, and dropping on the glass walll!! the stirring speedis minimum for several minutes, after 10-15 mins we can try to speed it up a little, and obtain the control of 36c. when temp will be "slowly not incrashing" stirrin is adjusted to keep 36c, usually it can be about 700-900 RPM using 2 leaf stirrer. Flask size is 250 ml for that scale.

TLC is performed to check of remains of 2b4m, if cant be performed the best sign is "deep yellow" is a sign that reaction is over, 4x volumetric amount of used dmso/nmp is added to the flask to stop the reaction.

Now its time to get rid of methylamine by 3x wash with cold h2o and begin to acidfiication using h2o and acid. After that solvent is evaporated.

 

[Russian lab assistant]

Can you tell me why to mix DCM and NMP? Does it improve the process? Why not just use DCM as usual? Is there any benefit?

 

[Dr. MMX]

The example of this technique was posted by HerrHaber here: http://bbzzzsvqcrqtki6umym6itiixfhn.../pl/threads/improved-synthesis-of-4mmc.13263/

http://bbzzzsvqcrqtki6umym6itiixfhni37ybtt7mkbjyxn2pgllzxf2qgyd.onion/pl/threads/improved-synthesis-of-4mmc.13263/

 

[Russian lab assistant]

Can you tell me why to mix DCM and NMP? Does it improve the process? Why not just use DCM as usual? Is there any benefit?

 

[Russian lab assistant]

Can you tell me why to mix DCM and NMP? Does it improve the process? Why not just use DCM as usual? Is there any benefit?

 

[rotovap5002]

It decreases synth time

 

[Russian lab assistant]

for how long?

 

[achemica2500]

how about toluene what's his use(he replace what) ,and how ,time,boiling,how to add and when....?

 

[Russian lab assistant]

toluene. Absolutely the same recipe...more output! But it stinks very badly. The main thing is not to use commercial toluene, only laboratory grade

 

[TayRonz]

can the ratio between 2b4m and MA HCl be reduced?
because in this synthesis you use x5 times more moles of methylamine hcl than 2b4m