MDMA Synthesis: From PMK to Production Techniques

Synthesis of MDMA from Piperonylmethylketone (PMK)

MDMA, commonly known as Ecstasy or Molly, is a popular recreational drug known for its euphoric effects. While its use is illegal in many places, it is still produced illicitly. Below is a simplified guide to the synthesis of MDMA from Piperonylmethylketone (PMK), a precursor chemical.

Reaction scheme:

Equipment and Glassware

• 100 ml round bottom flask
• Retort stand and clamp for securing apparatus (optional)
• Reflux condenser
• Heating plate
• Funnel
• Syringe or Pasteur pipette
• pH indicator papers
• Beakers (250 mL x2, 100 mL x4)
• Vacuum source
• Laboratory scale (0.01-100 g is suitable)
• Measuring cylinders 10 mL and 100 mL
• Water bath
• Glass rod and spatula
• Separatory funnel 0.5 L
• Laboratory grade thermometer (up to 200-250 °C)
• Buchner flask and funnel
• Filter paper

Reagents

• Formic acid 10.98 g
• n-Methylformamide (NMF; CAS 123-39-7) 7.6 g
• MDP2P (PMK; CAS 4676-39-5) 9.0 g
• Concentrated hydrochloric acid (HCl 36%) 30 ml
• Sodium hydroxide solution (NaOH 35%) ~10 ml
• Diethyl ether (or petroleum ether) ~150 ml
• Magnesium sulfate (MgSO4) ~15 g
• Methanol (MeOH) ~50 ml
• Acetone ~50 ml

Synthesis Steps

1. Place 3.66 g of formic acid, 7.6 g of n-methylformamide (NMF), and 9.0 g of MDP2P (PMK) into a 100 ml round bottom flask. Install a reflux condenser and thermometer.
2. Reflux the mixture at 150-170 °C for 7 hours with periodic additions of 7.32 g of formic acid.
3. After refluxing, cool the reaction mixture to room temperature to obtain a clear yellow solution of N-formyl-3,4-methylenedioxymethylamphetamine (N-formyl-MDMA). Wash this solution with distilled water twice and dry it over MgSO4. Filter out any solids.
4. Add 30 ml of concentrated hydrochloric acid (HCl 36%) to the solution. Heat the mixture at 80 °C for an additional 3 hours.
5. Alkalize the reaction mixture with several portions of sodium hydroxide solution (NaOH 35%) to achieve a pH of 12. Be cautious not to overheat the mixture.
6. Extract the crude MDMA free base from the alkaline solution with diethyl ether (or petroleum ether) using 2 x 50 mL portions. Dry the ether extract containing MDMA free base over MgSO4.
7. Evaporate the organic solvent with slight heating using a warm water bath or a rotary evaporator under vacuum. This will yield MDMA free base oil, which can then be converted to MDMA hydrochloride.
8. Treat the MDMA free base oil with hydrogen chloride gas to obtain a gelatinous brown precipitate of impure MDMA hydrochloride.
9. Dissolve the crude MDMA hydrochloride salt in the minimum volume of boiling methanol (MeOH) required for dissolution. Pour the hot solution into a beaker with chilled acetone to form crystals. Cool the mixture to room temperature, vacuum filter, wash the crystals with a small amount of cold dry acetone, and air dry (or dry in a vacuum chamber) to obtain crystalline MDMA hydrochloride.
10. Optionally, recrystallize MDMA hydrochloride once more to obtain fawn crystals with a melting point of 147 - 148 °C.