Mephedrone Synthesis of mephedrone (4-MMC) in NMP solvent. Large scale.

[ireshop]

Reaction Scheme:

Reagents:

• 2-Bromo-4'-methylpropyrophenone (cas 1451-82-7) - 5 kg
• N-Methyl-2-pyrrolidone (NMP; cas 872-50-4) - 20 L
• Methylamine 40% aqueous solution (cas 74-89-5) - 8 L
• Benzene - 20 L
• Acetone - 30 L
• Hydrochloric acid concentrated aqueous sol. (HCl 36%) ~ 1.5 l
• Distilled water - 20 L
• Magnesium sulphate (MgSO4)

Laboratory equipment and materials:

• 100 L batch reactor, equipped with dropping funnel, overhead stirrer, thermometer, temperature control system (cooling) and reflux condenser.
• Funnel
• pH indicator papers
• Several 25 L buckets
• 100 L drum
• 2000 mL beaker
• Vacuum source
• Balance
• 1000 mL measuring cylinder
• Glass rod and spatula
• Paddle
• Nutsche filter
• Rotary evaporator

Synthesis procedures

1. 5 kg 2-Bromo-4'-methylpropyrophenone or any other crude amount of 2-Bromo-4'-methylpropyrophenone after halogenation reactions is poured into the batch reactor.
2. Pour 20 L of N-methyl-2-pyrrolidone into the reactor. The upper stirrer is switched on and the reaction mixture is heated up to 40 °C.
3. When the temperature of 40 °C is reached, a 40 % aqueous methylamine solution of 8 L is poured into the reaction mixture and stirred for 20 min.
4. Then 20 L of cold distilled water is poured into the reaction mixture and stirred for a few 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. Then the stirrer is stopped, and the mixture is divided into two layers.
7. The lower aqueous layer is drained through the lower valve of the reactor. The upper layer is drained into a bucket and dried with MgSO4. The dried solution is then poured into another bucket.
8. Cold 20 L acetone is added to the reaction mixture and hydrochloric acid (HCl 36%) is added dropwise with constant stirring until a pH of 5.5-6 is reached.
9. The mixture is placed in a freezer for 12 hours.
10. The crystallised mephedrone hydrochloride is filtered through a Nutsche filter and air dried. The yield is 58 %.

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

 

[mcdonalds]

finally ! a forum in spanish !!!. i think it's great.

According to the final note NMP can be substituted by DMSO, DMF, Sulfolane.

So we should understand that following the tutorial we will substitute the 20 Litres of NMP by 20 L of any of the three DMSO, DMF, Sulfolane.

Best regards

 

[ireshop]

Hi mate !

Yes, any of the three would be valid.