Reaction scheme:
Reagents:
- Methylamine 40% aq (cas 74-89-5) 2 ml;
- Ethanol (EtOH) 5 ml;
- 3,4-Methylenedioxyphenylpropan-2-one (MDP2P; PMK; cas 4676-39-5) 2 ml;
- Adams' catalyst (PtO2; cas 1314-15-4) 0.05 g;
- Distilled water 165 ml;
- Hydrochloric acid (36% aq HCl);
- Dichloromethane 450 ml;
- Dodium hydroxide solution (25% aq NaOH);
- MgSO4 anhydrous;
- Isopropyl alcohol (IPA) ~50 ml;
- Diethyl ether ~50 ml;
Equipment and glassware:
- Pear shaped flask 10 ml;
- Retort stand and clamp for securing apparatus (optional);
- Hydrogen gas (H2) source;
- Vessel for height pressure reaction with manometer (thick glass champagne bottle can be modified for this synthesis);
- Hoses;
- Syringe or Pasteur pipette;
- pH indicator papers;
- Beakers (50 mL x2, 100 mL x2);
- Laboratory scale (0.1-200 g is suitable);
- Measuring cylinder 10 mL;
- Glass rod and spatula;
- Separatory funnel 0.5 L (optional);
- Buchner flask and Schott funnel;
- Vacuum in desiccator (optional);
- Rotary evaporator (optional);
1. Methylamine 40% aq 2 ml is added to ethanol (EtOH) 5 ml.
2. 3,4-Methylenedioxyphenylpropan-2-one (MDP2P; PMK) 2 ml is slowly poured into the mixture and stirred for 1 h at room temperature.
3. Adams' catalyst (PtO2) 0.05 g is added to the mixture under nitrogen flow.
4. Reaction mixture is placed under a hydrogen atmosphere at 56 psi (3.86 bar) for 3.5 h.
5. The pressure have to be returned to 56 psi at the 1 and 2 h of exposure in the vessel.
6. A reek and PtO2 is removed in vacuum after filtration through Celite with ethanol.
7. The residue is dissolved in distilled water 165 ml and acidified with hydrochloric acid (36% aq HCl) to pH 1. Then, extracted with DCM (3x75 ml).
8. The aqueous phase is alkalized with sodium hydroxide solution (25% aq NaOH) to pH 10 and organic substances are extracted with DCM (3x75 ml).
9. Additional sodium hydroxide solution (NaOH aq 25%) 10 and 20 drops are added before the second and third DCM extractions respectively.
10. Combined organic layers are dried over MgSO4 anhydrous and concentrated in vacuum to give clean amber MDMA free base oil. The yield is 2.0 g (~76 %).
11. MDMA free base oil 2 g is dissolved in isopropyl alcohol (IPA) 3.5 ml and acidified with hydrochloric acid (HCl aq 36 %) ~40 drops to reach pH 5.5-6.
12. The solvent is removed under vacuum with heat, a precipitate is formed (color range from white to pink and to brown). The precipitate of MDMA hydrochloride is homogenized and washed with a IPA:ether 2:1 solution before a final washing with ether on Buchner flask and Schott funnel.
13. The resulting white MDMA hydrochloride is dried under vacuum in desiccator. The yield is 2.3 g (total yield ~73 %).
2. 3,4-Methylenedioxyphenylpropan-2-one (MDP2P; PMK) 2 ml is slowly poured into the mixture and stirred for 1 h at room temperature.
3. Adams' catalyst (PtO2) 0.05 g is added to the mixture under nitrogen flow.
4. Reaction mixture is placed under a hydrogen atmosphere at 56 psi (3.86 bar) for 3.5 h.
5. The pressure have to be returned to 56 psi at the 1 and 2 h of exposure in the vessel.
6. A reek and PtO2 is removed in vacuum after filtration through Celite with ethanol.
7. The residue is dissolved in distilled water 165 ml and acidified with hydrochloric acid (36% aq HCl) to pH 1. Then, extracted with DCM (3x75 ml).
8. The aqueous phase is alkalized with sodium hydroxide solution (25% aq NaOH) to pH 10 and organic substances are extracted with DCM (3x75 ml).
9. Additional sodium hydroxide solution (NaOH aq 25%) 10 and 20 drops are added before the second and third DCM extractions respectively.
10. Combined organic layers are dried over MgSO4 anhydrous and concentrated in vacuum to give clean amber MDMA free base oil. The yield is 2.0 g (~76 %).
11. MDMA free base oil 2 g is dissolved in isopropyl alcohol (IPA) 3.5 ml and acidified with hydrochloric acid (HCl aq 36 %) ~40 drops to reach pH 5.5-6.
12. The solvent is removed under vacuum with heat, a precipitate is formed (color range from white to pink and to brown). The precipitate of MDMA hydrochloride is homogenized and washed with a IPA:ether 2:1 solution before a final washing with ether on Buchner flask and Schott funnel.
13. The resulting white MDMA hydrochloride is dried under vacuum in desiccator. The yield is 2.3 g (total yield ~73 %).
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