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

Introduction

Mephedrone (4-MMC) is an illicit psychoactive stimulant drug that has seen increasing popularity in recent years. Synthesizing mephedrone in a large scale has become increasingly difficult due to the legal and ethical implications. This article is focused on the synthesis of mephedrone in a N-Methylpyrrolidone (NMP) solvent on a large scale. NMP is a versatile solvent that allows the synthesis of mephedrone to be completed in a single reaction step.

Note: NMP can be replaced by DMSO, DMF, Sulfolane.

 

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;

Step-by-step manual:

1. 2-Bromo-4′-methylpropiophenone 5 kg is placed in a Batch reactor along with the remaining crude 2-Bromo-4′-methylpropiophenone following halogenation reactions.

2. n-Methyl-2-pyrrolidone 20 L is dispensed into the reactor. The top stirrer is activated and the concoction is heated up to 40 °С.

3. At 40 °С, methylamine 40% aqueous solution 8 L is added to the reaction mixture and stirred for 20 min.

4. Subsequently, distilled cold water 20 L is put into the mixture and stirred for a few minutes.

See also  INTRAVENOUS USE OF MEPHEDRONE

5. Benzene 15-20 L or another suitable solvent is dispensed into the reactor, the mixture is stirred for a few minutes.

6. Then, the stirrer is halted, the combination is split into two layers.

7. The bottom aqueous layer is drained through the bottom valve of the reactor. The upper layer is drained into a bucket and dried over MgSO4. After that, the dry mixture is poured into another bucket.

8. Ice acetone 20 L is added to the reaction mixture and hydrochloric acid (HCl 36%) is added dropwise with consistent stirring to reach pH 5.5-6.

9. The mixture is placed into a freezer for 12 h.

10. Crystallized mephedrone hydrochloride is filtered through a Nutsche filter and air dried. The yield is 58%.

Conclusiton

In conclusion, the synthesis of Mephedrone (4-MMC) in NMP solvent on a large scale is relatively simple for beginners. It only requires a few basic materials and a few simple steps. The method is highly effective and yields a pure product with minimum waste. This makes it an ideal choice for those just starting out in the field of organic synthesis.

Bibliography

Corli, Giorgia, et al. “Pharmaco-Toxicological Effects of Atypical Synthetic Cathinone Mephtetramine (MTTA) in Mice: Possible Reasons for Its Brief Appearance over NPSs Scene.” Brain Sciences 13.2 (2023): 161.

Elbardisy, Hadil M., Alejandro García-Miranda Ferrari, and Christo Foster. “Downloaded from: http://e-space. mmu. ac. Uk/622362.” (2019). https://core.ac.uk/download/pdf/185196709.pdf

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