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Mephedrone Synthesis of mephedrone (4-MMC) using NMP solvent (in large quantities)

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Reaction diagram


Reagents
  • 2-Bromo-4'-methylpropiophenone (case 1451-82-7) - 5 kg;
  • N-methyl-2-pyrrolidone (NMP; case 872-50-4) or DMSO, DMF, Sulfolane - 20 L;
  • Methylamine 40% aqueous solution (case 74-89-5) - 8 L;
  • Benzene - 20 L;
  • Acetone - 30 L;
  • Hydrochloric acid in aqueous solution (HCl 36%) ~ 1.5 L;
  • Distilled water - 20 L;
  • Magnesium sulfate (MgSO4);




Equipment and glassware

  • Batch reactor equipped with drop funnel, top stirrer, thermometer, temperature control system and reflux condenser;
  • pH indicator paper;
  • A balance
  • Vacuum pump;
  • Funnel;
  • Several buckets - 25 L;
  • Barrel -100 L;
  • Beaker - 2000 mL;
  • Test tube - 1000 mL;
  • Glass rod and spatula;
  • Spoons;
  • Nutsche filter;
  • Rotary evaporator;



Synthesis procedures

  1. 5kg of 2-Bromo-4'-methylpropiophenone (or other crude 2-Bromo-4'-methylpropiophenone after halogenation reactions) is poured into the batch reactor.
  2. Next, 20 L of N-methyl-2-pyrrolidone is poured into the reactor. Switch on the top stirrer and heat the reaction mixture to 40 °С.
  3. When the temperature reaches 40 °С, 8 L of methylamine 40% aqueous solution is poured into the mixture and mixed for 20 minutes.
  4. Afterwards, 20 L of distilled water is placed in the reaction mixture and stirred for several minutes.
  5. 15-20 L of benzene or other suitable solvent is poured into the reactor, and the mixture is stirred for a few minutes.
  6. When the stirrer stops, the mixture is divided into 2 layers.
  7. The lower aqueous layer is discharged through the bottom valve of the reactor. The upper layer is drained into a bucket and dried with MgSO4. This is then poured into another bucket.
  8. 20 L of ice-cold acetone is added to the mixture, and hydrochloric acid (HCl 36%) is added dropwise with constant stirring to achieve a pH of 5.5-6 .
  9. The mixture is placed in the freezer for around 12 hours.
  10. The crystallized mephedrone hydrochloride is then filtered and air-dried. The yield is 58%.




Source: William Dampier ( /media/mephedrone-hydrobromide-synthesis.57/ )
 
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