WillD
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Reagents:
Step 2. Beta-nitro-3,4,5-trimethoxystyrene reduction with NaBH4/CuCl2 to mescaline.
- 3,4,5-Trimethoxybenzaldehyde (cas 86-81-7) 1000 g;
- Acetic acid 5 L;
- Nitromethane (cas 75-52-5) 2 L;
- Cyclohexylamine (cas 108-91-8) 100 ml;
- Distilled water ~17 L;
- Isopropyl alcohol (IPA) ~23 L;
- Sodium borohydride (NaBH4) 1200 g;
- Copper chloride (CuCl2) 72 g;
- Sodium hydroxide (NaOH) 25% aq. 8 L;
- Magnesium sulfate (MgSO4);
- Acetone 2.5 L;
- Sulfuric acid (H2SO4 conc.) ~410 mL or hydrochloric acid (HCl conc.) ~150 mL;
- Round bottom flask 20 L;
- Batch reactor 50 L equipped with drip funnel, top stirrer, reflux condenser and heating system;
- Retort stand and clamp for securing apparatus;
- Top stirrer;
- Boiling chips;
- Reflux condenser;
- Glass rod and spatula;
- Heating plate;
- Laboratory grade thermometer;
- Laboratory scale (1-1000 g is suitable);
- Measuring cylinders 100 mL and 1 L;
- Funnel;
- Filter paper;
- Rotovap machine;
- Vacuum source;
- Buchner flask (large) and funnel;
- pH Indicator paper;
- Beakers 1000 ml x2 and 2000 ml x2;
- Several buckets;
- Freezer;
1. 3,4,5-Trimethoxybenzaldehyde (cas 86-81-7) 1000 g , acetic acid 5 L and nitromethane 2 L are added into a 20 l flask.
2. The reaction mixture is stirred and cyclohexylamine 100 ml is added.
3. The mixture is heated to 80 °C and stirred for 3 h.
4. Distilled water 10 L is added dropwise with constant stirring. Yellow crystals are formed.
5. Crystals are filtered and washed with distilled water.
6. Then, they are air dried at room temperature.
7. Next, crystals are dissolved in boiling hot IPA (as minimum as possible) and put into a freezer for 12 h.
8. Crystals are filtered, washed with a small amount of cold IPA and air dried after the solution crystallization procedure 7. Beta-nitro-3,4,5-trimethoxystyrene (cas 6316-70-7) yield is 920 g.
2. The reaction mixture is stirred and cyclohexylamine 100 ml is added.
3. The mixture is heated to 80 °C and stirred for 3 h.
4. Distilled water 10 L is added dropwise with constant stirring. Yellow crystals are formed.
5. Crystals are filtered and washed with distilled water.
6. Then, they are air dried at room temperature.
7. Next, crystals are dissolved in boiling hot IPA (as minimum as possible) and put into a freezer for 12 h.
8. Crystals are filtered, washed with a small amount of cold IPA and air dried after the solution crystallization procedure 7. Beta-nitro-3,4,5-trimethoxystyrene (cas 6316-70-7) yield is 920 g.
Step 2. Beta-nitro-3,4,5-trimethoxystyrene reduction with NaBH4/CuCl2 to mescaline.
1. Isopropanole-water mixture (IPA/H2O 2:1) 18 L is added to a 50 L batch reactor.
2. Sodium borohydride (NaBH4) 1200 g is added in one portion at a constant stirring.
3. Beta-nitro-3,4,5-trimethoxystyrene (cas 6316-70-7) 1000 g is added in small portions so that the mixture temperature is kept below 60 °C.
4. Copper chloride (CuCl2) 72 g in distilled water 200 ml is added dropwise so that the mixture temperature is kept below 80 °C.
5. Thereafter, the reaction mixture is held at 80 °C for 30 min with help of an external heating.
6. Sodium hydroxide 25% water solution (NaOH) 8 L is added to the reaction mixture, mixed well. Obtained layers are separated.
7. The aqueous layer is extracted with IPA 8 L (or DCM, or ether, or benzene). Extracts are combined and dried over magnesium sulphate (MgSO4).
8. Solvent is distilled off under reduced pressure to an oil.
9. The oil is dissolved in dry acetone 2 L.
10. Sulfuric acid (H2SO4 conc.) or hydrochloric acid (HCl conc.) is added dropwise with a constant stirring to reach pH 6.
11. The mixture is put into the freezer for 12 h.
12. The suspension is filtered and washed with a dry cold acetone after crystallization procedure. Mescaline (cas 642-73-9 or cas 832-92-8) yield is 60-70%.
2. Sodium borohydride (NaBH4) 1200 g is added in one portion at a constant stirring.
3. Beta-nitro-3,4,5-trimethoxystyrene (cas 6316-70-7) 1000 g is added in small portions so that the mixture temperature is kept below 60 °C.
4. Copper chloride (CuCl2) 72 g in distilled water 200 ml is added dropwise so that the mixture temperature is kept below 80 °C.
5. Thereafter, the reaction mixture is held at 80 °C for 30 min with help of an external heating.
6. Sodium hydroxide 25% water solution (NaOH) 8 L is added to the reaction mixture, mixed well. Obtained layers are separated.
7. The aqueous layer is extracted with IPA 8 L (or DCM, or ether, or benzene). Extracts are combined and dried over magnesium sulphate (MgSO4).
8. Solvent is distilled off under reduced pressure to an oil.
9. The oil is dissolved in dry acetone 2 L.
10. Sulfuric acid (H2SO4 conc.) or hydrochloric acid (HCl conc.) is added dropwise with a constant stirring to reach pH 6.
11. The mixture is put into the freezer for 12 h.
12. The suspension is filtered and washed with a dry cold acetone after crystallization procedure. Mescaline (cas 642-73-9 or cas 832-92-8) yield is 60-70%.
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