Mephedrone synthesis (4-MMC) in NMP solvent. Large scale.

WillD

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Reaction scheme:
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Reagents:
  • 2-Bromo-4'-methylpropiophenone (cas 1451-82-7) - 5 kg;
  • n-Methyl-2-pyrrolidone (NMP; cas 872-50-4) - 20 L;
  • Methyl amine 40% aq. solution (cas 74-89-5) - 8 L;
  • Benzene - 20 L;
  • Acetone - 30 L;
  • Hydrochloric acid con. aq. solution (HCl 36%) ~ 1.5 L;
  • Distilled water - 20 L;
  • Magnesium sulphate (MgSO4);

Equipment and glassware:
  • 100 L Batch reactor, which is equipped with drip funnel, top stirrer, thermometer, temperature control system (cooling) and reflux condenser;
  • Funnel;
  • pH indicator papers;
  • Several buckets 25 L;
  • Barrel 100 L;
  • Beaker 2000 mL;
  • Vacuum source;
  • Scale;
  • Measuring cylinder 1000 mL;
  • Glass rod and spatula;
  • Scoops;
  • Nutsche filter;
  • Rotary evaporator;

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Synthesis procedures
1. 2-Bromo-4'-methylpropiophenone 5 kg is poured into Batch reactor or another crude 2-Bromo-4'-methylpropiophenone amount after halogenation reactions.
2. n-Methyl-2-pyrrolidone 20 L is poured into the reactor. Top stirrer is turned on and the reaction mixture is heated up to 40 °С.
3. When temperature is reached 40 °С, methylamine 40% aq. solution 8 L is poured into the reaction mixture and stirred for 20 min.
4. Next, distilled cold water 20 L is poured into reaction mixture and stirred for few minutes.
5. Benzene 15-20 L or other suitable solvent is poured into the reactor, the mixture is stirred for few minutes.
6. Than, the stirrer is stopped, the mixture is divided into two layers.
7. The bottom aqueous layer is drained through the bottom valve of the reactor. Top layer is drained into a bucket and dried over MgSO4. Than, dry solution is poured in another bucket.
8. Ice acetone 20 L is added to the reaction mixture and hydrochloric acid (HCl 36%) is added dropwise with a constant stirring to reach pH 5.5-6.
9. The mixture is put into a freezer for 12 h.
10. Crystallized mephedrone hydrochloride is filtered on a Nutsche filter and air dried. The yield is 58%.


Note
NMP can be replaced by DMSO, DMF, Sulfolane.
 
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Hans-Dietrich

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How about synthesis in DСM ?
 

BHBlueberry

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Wow it looks so easy.. If I only would like meph I would play with this formula ;)
 

dark_side_of_chemistry

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thanks . I have access to 2b3ch but liquid. i understand he is already in some solvent, right?
 

dark_side_of_chemistry

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OK I understand . so should I mix it one to one with dsmo?
 

dark_side_of_chemistry

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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.
 

dark_side_of_chemistry

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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

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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.
 

dark_side_of_chemistry

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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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ASheSChem

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noob question;
we need to keep the bottom layer or the one above ? :x
 

WillD

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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)
 

Marocamora

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Mr William please does mephedrone look very much like cocaine and does it have the same effects? And if it is put in the tongue it causes the tongue to be like cocaine? thank you.
 
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deploy

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It's a stimulant, not an anesthetic
 

BitcoinScam

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no if you mix with licodaine or benzocaine then he will get effect like cocaine
 

GaDjo

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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

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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)
 

Selassi

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How many methylamine did u end up using in the cmc-synth?
 
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