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Synthesis of mephedrone in NMP (large scale)

William Dampier

Active member
Expert
Reaction scheme:
UeWf0vGO6N.png


Reagents:

2-bromo-4-methylpropiophenone (BK4) - 5 kg;
n-methyl-2-pyrrolidone (NMP) - 20 L;
Methyl amine 40% aq.soln - 8 L;
Benzene - 15 L;
Acetone - 30 L;
Hydrochloric acid con.aq.soln ~ 1,5 L.

Synthesis:
1. 5 kg 2-bromo-4-methylpropiophenone (BK4) added to the reactor or have calculated amount of crude BK4 after halogenation reactions.
2. 20 liters n-methyl-2-pyrrolidone poured, start stirring and heating to 40 *C.
3. Upon reaching 40 *C within the mixture, pour 8 liters methyl amine 40% aq.soln and continue stirring 20 minutes.
4. Next, we pour 20 liters of clean cold water, stirring a few minutes.
5. Pour 15-20 liters benzene or other suitable extractor, stirring a few minutes.
6. Stop stirring, waiting for the separation of the mixture into two layers.
7. The bottom aqueous layer was drained through the bottom valve of the reactor.
8. 20 liters of ice acetone was poured and add hydrochloric acid with stirring to pH - 5
9. Overload the mixture in the freezer.
10. Filter on the nutshe-filter, dry.

Notes:
NMP can be replaced by DMSO, DMF, Sulfolane.
 
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William Dampier

Active member
Expert
OK I understand . so should I mix it one to one with dsmo?
NMP 4:1 min amount. If u have large barrel, u can add proportions, it's better for reaction.
what do you think to carry out this reaction in such a tank? 115l. I thought to wrap it with a heating belt and install a mechanical stirrer in advance

wrapped in such a heating mantle that you can heat the reactions up to 55 degrees
Good
 
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Somehow, close the upper inlet and let the methylamine drain out so as not to burst the tank, or it is better to leave it open, install only the thermometer and the stirrer.
 
is this recipe not given the wrong methylamine value? there should be no more than 8l for hot synthesis? Should this excess of methylamine be smaller during the synthesis in nmp?
 

KHaafii

New member
How much end product do you end up with this Synthesis approximately with this recipe. For how much does uncut/Pure mephedrone go away on the market per kg? How much profit margin is there in mephedrone. Doesn't have to be petty exactly but approximately.

I have no knowledge in the market of mephedrone on a large scale. I have read that this is also fairly in demand? I don't mean for users but people who buy this for their own reasons on larger numbers.
 
one question as to the amount of methylamine used in this reaction. 8l is enough for 5kg of bk4? my calculations show that 14.8l is needed.

counting process: for 1mol of bk4 we need 5mol of methylamine. 5kg bk = 5000g. 5000g / 227g = 22mol bk4. 22 mol x 5 = 110 mol methylamine. 110mol = 3416.6g ... I did 33% times because a 40% aqueous solution never has that many percent. 10353g or 14790ml of an aqueous solution of methylamine comes out ...

these 8l of methylamine is about three times the bk4. my calculations are with a fivefold excess ... threefold is enough?
 
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William Dampier

Active member
Expert
How much end product do you end up with this Synthesis approximately with this recipe. For how much does uncut/Pure mephedrone go away on the market per kg? How much profit margin is there in mephedrone. Doesn't have to be petty exactly but approximately.

I have no knowledge in the market of mephedrone on a large scale. I have read that this is also fairly in demand? I don't mean for users but people who buy this for their own reasons on larger numbers.
The demand and prices depend on the volume of purchases of the wholesale of raw materials and your region. This synthesis is well suited for production in large quantities (ton per month and more)
 

GaDjo

New member
Hello
I am a beginner and want to start with this synthesis. You advise me to synthesize the precursors myself or to buy them (for example on fischersci)? I want a small production, 20g maximum
 

GaDjo

New member
Hello,
For me it is shit not synthesis. Someone tried it ? What is the yield ? Your final product will kristalized in solution of benzene and acetone ? What next, washing it by acetone ? What form has the Cristals ... ?
For crystallization, you need a final step. Put you mephedrone powder on 70% Ethanol/30% H2O (1g of mephedrone for 3ml). Boil it. Poor on crystallization dishes. Wait the evaporation of ethanol and water. You've get your meph' crystals
more water you have in your solution, more your rocks will be big
(recipe found on /d/drugmanufacture, not tested)
 
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