Reaction scheme:
- 100 ml round bottom flask;
- Retort stand and clamp for securing apparatus (optional);
- Heating plate;
- Funnel;
- Syringe or Pasteur pipette;
- pH indicator papers;
- Beakers (250 mL x2, 100 mL x4);
- 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 sulphate (MgSO4) ~15 g;
- Methanol (MeOH) ~50 ml;
- Acetone ~50 ml;
Synthesis:
1. Formic acid 3.66 g, n-methylformamide (NMF) 7.6 g and MDP2P (PMK) 9.0 g are placed into a 100 ml round bottom flask. Reflux condenser and thermometer are installed.
2. The mixture is refluxed at 150-170 °C for 7 h with periodic formic acid 7.32 g additions.
3. After that, the reaction mixture is cooled down to room temperature, a clear yellow solution of N-formyl-3,4-methylenedioxymethylamphetamine (N-formyl-MDMA) is obtained. N-formyl-MDMA solution have to be washed with distilled water twice and dried over MgSO4. Dry solution is filtered from solids.
4. Concentrated hydrochloric acid (HCl 36% 30 ml) is added to this solution. Than, reaction mixture is heated at 80 °C for additional 3 h.
5. The reaction mixture is alkalized with several portions of sodium hydroxide solution (NaOH 35%) to 12 pH. Do not overheat reaction mixture.
6. Crude MDMA free base is extracted from the alkaline solution with diethyl ether (or petroleum ether) 2 x 50 mL. Ether extract with MDMA free base is dried over MgSO4.
7. After that, organic solvent is evaporated with a slight heating of warm water bath or with help of rotary evaporator with vacuum. MDMA free base oil is treated with hydrogen chloride gas and gelatinous brown precipitate of impure MDMA hydrochloride is obtained.
8. The crude MDMA hydrochloride salt is dissolved in minimum volume of boiling methanol (MeOH), which is necessary to dissolve MDMA crude salt. Hot solution is poured into a beaker with chilled acetone, crystals are formed. This mixture is cooled down to a room temperature and vacuum filtered, crystals are washed with small amount of cold dry acetone and air dried (or dried in a vacuum chamber). Crystalline MDMA hydrochloride is obtained as the product.
9. MDMA hydrochloride can be recrystallized one more time to yield fawn crystals with melting point 147 - 148 °C.
2. The mixture is refluxed at 150-170 °C for 7 h with periodic formic acid 7.32 g additions.
3. After that, the reaction mixture is cooled down to room temperature, a clear yellow solution of N-formyl-3,4-methylenedioxymethylamphetamine (N-formyl-MDMA) is obtained. N-formyl-MDMA solution have to be washed with distilled water twice and dried over MgSO4. Dry solution is filtered from solids.
4. Concentrated hydrochloric acid (HCl 36% 30 ml) is added to this solution. Than, reaction mixture is heated at 80 °C for additional 3 h.
5. The reaction mixture is alkalized with several portions of sodium hydroxide solution (NaOH 35%) to 12 pH. Do not overheat reaction mixture.
6. Crude MDMA free base is extracted from the alkaline solution with diethyl ether (or petroleum ether) 2 x 50 mL. Ether extract with MDMA free base is dried over MgSO4.
7. After that, organic solvent is evaporated with a slight heating of warm water bath or with help of rotary evaporator with vacuum. MDMA free base oil is treated with hydrogen chloride gas and gelatinous brown precipitate of impure MDMA hydrochloride is obtained.
8. The crude MDMA hydrochloride salt is dissolved in minimum volume of boiling methanol (MeOH), which is necessary to dissolve MDMA crude salt. Hot solution is poured into a beaker with chilled acetone, crystals are formed. This mixture is cooled down to a room temperature and vacuum filtered, crystals are washed with small amount of cold dry acetone and air dried (or dried in a vacuum chamber). Crystalline MDMA hydrochloride is obtained as the product.
9. MDMA hydrochloride can be recrystallized one more time to yield fawn crystals with melting point 147 - 148 °C.
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and there is not advantage if you crystal in fridge