Question Mephedrone synthesis - amination in DCM or NMP? - Please discuss here

[eps0n]

What will give better yields? I have been talking to some people and there is conflicting opinions. In my opinion doing the amination in NMP will give more yield since the reaction is faster and the freebase mephedrone will not break down. But others said that DCM will give same yields, or even that NMP gives lower yield.

Some expert opinion would be great!

Or just discuss and state your viewpoints

 

[yin-yang]

There are certain occurrence in science which contradict well establish theory and no one knows why. Only way to know for sure is through experiment.

Do you have bk4, meAmine and common solvents (Ethyl acetate, NMP, DMSO...)If so, small scale would be ideal with standardized comparison between the samples. Maybe some will yield
better but what is that good for if the products is heavily contaminated and doesn't perform well? 4mmc is relatively "new" so all of us are pioneers in perfecting this synth. This will encourage others to indulge in research as well.

 

[Netflix]

on a small scale it is much better to produce for a large scale because it is difficult to detect such a labore and you can produce without problems with the police for years. large labs are quickly caught and you will have years in jail.
I made 7 years 4mmc on dcm and it is much easier to synthesize, because there are no lab equipment, the same bottles of juice. syringe and cloth for furniture. and made it easy with 100g 2b4m 60g-70g of crystals. every day 24 days x 60g-70g = 1.440g-1.680g x 20 € a very good month.

 

[yin-yang]

If someone is going to sell, much better option is to make stockpile and perform this reaction on big scale inside 200l plastic barrel with hand mortar mixer coated in teflon and some cooling system in place. Luckly it's easy to dispose equpment. Separate manifaturing and distribution part as chemists are on top of food chan and everybody will rat on them.

How was your product? What was the feedback from customers? Did you ever use any other solvent, any difference in qualaty? DCM is hard to get rn due to EU regulations..

 

[Netflix]

yes toulen i used. dcm is very well available in eu. 97% purity tested in Barcelona. when you have a barrel open it smells very much and the smell alone can make you have trouble with your neighbors. if you close the barrel tightly, the pressure will burst it.

 

[eps0n]

For how long do you let it react? In scientific literature ideal method is 55-60 °C for 10 minutes:

"In an effort to find other reaction conditions for step 2 3a, we searched the literature for
syntheses of a-tert-butylaminopropiophenone, the ring-unsubstituted analog of bupropion.

We found only one reference 9 to the synthesis of this compound, and it prescribed 5 hours reflux in benzene and resulted in only a 37% yield.

We then tried N-methylpyrrolidinone (NMP) as a solvent and found that the reaction t-butyl amine and 2 at room temperature in this solvent was noticeably exothermic and went to completion (as judged by disappearance of 2 by GC-MS) in less than 0.5 hours.

Out of consideration for the impatience of youth, we tried warming the reaction in a 60 (C water bath and found it was complete in less than 10 min.

By contrast, when the reaction is carried out in acetonitrile, the solvent used by the BW workers, it is not exothermic, considerably slower, and according to Hill et al. (7) resulted in only a 43% yield, while our yields averaged 75-85%."

This is about the synthesis of Bupropion, but I strongly believe the same can be applied to 4-MMC as the structure does not differ a lot. Considering posted yields with DCM are reported high, the same conditions most likely apply to DCM.

It would be a great contribution to our community if anyone has TLC plates and is willing to test for how long you need to run the reaction under different conditions (20 °C, 60 °C, DCM, NMP)