Introduction
Hydrolysis of BMK glycidate ethers is represented in this topic. The procedure is the same for ethyl (Et) [cas 41232-97-7] and methyl (Me) [cas 80532-66-7] esters of glycidic acid. In case of sodium (Na) salt of this acid [cas 5449-12-7], you can skip first stage of NaOH addition and start from acid hydrolysis. In addition, purification method of obtained P2P is described. This procedure have to be committed to get pure Phenylacetone (P2P) for further syntheses of methamphetamine or amphetamine.
Suppliers of BMK glycidate ethers can be found in BB Listing.
Difficulty rating: 2/10
Suppliers of BMK glycidate ethers can be found in BB Listing.
Difficulty rating: 2/10
Equipment and glassware:
- 1000 mL Round bottom flask;
- Reflux condenser;
- Retort stand and clamp for securing apparatus;
- pH indicator paper;
- Vacuum source (optional);
- Rotovap machine (optional);
- Glass rod and spatula;
- 100 mL x2; 250 mL x2; 500 mL x2 Beakers;
- Magnetic or top stirrer with a heating plate;
- Water bath;
- Funel;
- 1000 mL Separatory funnel;
- Vacuum distillation setup (optional);
Reagents:
- 100 g BMK glycidate ethers (cas 80532-66-7; cas 41232-97-7; cas 5449-12-7);
- ~20 g NaOH or KOH;
- ~80 ml HCl (35%) or 100 ml H2SO4 (45%);
- ~600 mL DCM or Petroleum Ether;
- ~100 g MgSO4 or Na2SO4;
- ~500-600 mL Distilled water;
- ~ 50 g NaCl (optional);
Hydrolysis of BMK glycidates
1. NaOH (or KOH) 20g is dissolved in 250-300 ml distilled water with stirring. The reaction mixture (Rm) have to be cooled to room temperature. BMK glycidate 100 g (methyl or ethyl ester) is added and dissolved completely. Part of BMK is hydrolyzed during this procedure and floated as an oil in the surface of Rm. Rm is stired for 1 h at 75-80 °C with a reflux condenser.
2. Then, 200 ml HCl (35%) or 240 ml H2SO4 (45%) are added in small portions to Rm and heated to 80-90 °C and stired for 3 h. Rm have to be cooled to room temperature, the precipitate is filtered.
3. The reaction solution is extracted with DCM or petroleum ether 3 x 100 ml. Extract is washed with brine to neutral pH 7 several times. Extract is dried with MgSO4 (or Na2SO4) (optional) and filtered from solids.
4. An organic solvent (DCM or petroleum ether) is distilled off to give 65 ml of P2P.
2. Then, 200 ml HCl (35%) or 240 ml H2SO4 (45%) are added in small portions to Rm and heated to 80-90 °C and stired for 3 h. Rm have to be cooled to room temperature, the precipitate is filtered.
3. The reaction solution is extracted with DCM or petroleum ether 3 x 100 ml. Extract is washed with brine to neutral pH 7 several times. Extract is dried with MgSO4 (or Na2SO4) (optional) and filtered from solids.
4. An organic solvent (DCM or petroleum ether) is distilled off to give 65 ml of P2P.
Phenylacetone (P2P) synthesis via BMK ethyl glycidate
P2P purification
1. The resulting phenylacetone (P2P) is transferred to a round bottom flask with distilled water 1:1 (w/w) and distilled with steam under vacuum.
2. Purified P2P from receiver flask is extracted from water mixture with DCM (or petroleuum ether) 3 x 100 mL. Extract is dried with MgSO4 (or Na2SO4).
3. The resulting solution is filtered from the solids (drying agent) and then an organic solvent is distilled off.
2. Purified P2P from receiver flask is extracted from water mixture with DCM (or petroleuum ether) 3 x 100 mL. Extract is dried with MgSO4 (or Na2SO4).
3. The resulting solution is filtered from the solids (drying agent) and then an organic solvent is distilled off.
Phenylacetone can be stored long time in a sealed vessel in a freezer. It is recommended to distill it before further syntheses of methamphetamine or amphetamine. Avoid direct sunlight onto phenylacetone and exposure to high temperatures.
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