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!