Reagents:
- Benzaldehyde 1000 g;
- Methyl ethyl ketone (MEK) 1000 ml;
- Distilled water 14.5 L;
- Chloroform (CHCl3) 7.6 L;
- Sodium bicarbonate solution (NaHCO3);
- Magnesium sulphate (Na2SO4) anhydrous;
- Glacial acetic acid 10 L;
- Hydrogen peroxide (H2O2) 1300 g 50 %;
- Sodium hydroxide (NaOH) 600 g;
Equipment and glassware:
- 5 and 10 L Round bottom flasks;
- Water bath;
- 25-30 L Batch reactor with reflux condenser and heating system;
- Glass rod and spatula;
- Rotovap machine (optional);
- pH indicator paper;
- Laboratory scale (1-1000 g is suitable);
- Measuring cylinders 1000 mL;
- 1000 mL x3; 2000 mL x3; 5000 mL x3 Beakers;
- Several buckets;
Step 1. 3-Methyl-4-phenyl-3-buten-2-one synthesis (cas 1901-26-4).
1. Benzaldehyde 1000 g and methyl ethyl ketone (MEK) 1000 ml are mixed in 5 L flask, stirred and chilled at 0 °C.
2. HCl gas is bubbled slowly through the mixture for a 1.5 h.
3. The solution is stirred for addition 1.5 h at room temperature.
4. Distilled water 2 L is added. The solution is extracted with chloroform (CHCl3) 800 ml x2, then the extract is washed with sodium bicarbonate solution (NaHCO3) to neutral pH and dried over magnesium sulphate (MgSO4).
5. Solvent is evaporated under vacuum and 3-methyl-4-phenyl-3-buten-2-one (cas 1901-26-4) is distilled under vacuum (b.p. 269.6±9.0 °C at 760 mm Hg). Reaction yield is 1000 g.
1. Benzaldehyde 1000 g and methyl ethyl ketone (MEK) 1000 ml are mixed in 5 L flask, stirred and chilled at 0 °C.
2. HCl gas is bubbled slowly through the mixture for a 1.5 h.
3. The solution is stirred for addition 1.5 h at room temperature.
4. Distilled water 2 L is added. The solution is extracted with chloroform (CHCl3) 800 ml x2, then the extract is washed with sodium bicarbonate solution (NaHCO3) to neutral pH and dried over magnesium sulphate (MgSO4).
5. Solvent is evaporated under vacuum and 3-methyl-4-phenyl-3-buten-2-one (cas 1901-26-4) is distilled under vacuum (b.p. 269.6±9.0 °C at 760 mm Hg). Reaction yield is 1000 g.
1. 3-Methyl-4-phenyl-3-buten-2-one (cas 1901-26-4) 1 kg from Step 1, glacial acetic acid 10 L and hydrogen peroxide (H2O2) 1300 g 50 % are poured into a 25-30 L batch reactor with reflux condenser, stirred and at 55 °C for 23 h.
2. Next, distilled water 10 L is added.
3. The reaction mixture is extracted with chloroform 5 L and dried over magnesium sulphate (Na2SO4).
4. Solvent is evaporated under vacuum. 2-Acetoxy-1-phenyl-1-propene (cas 24175-87-9) yield is 800 g.
2. Next, distilled water 10 L is added.
3. The reaction mixture is extracted with chloroform 5 L and dried over magnesium sulphate (Na2SO4).
4. Solvent is evaporated under vacuum. 2-Acetoxy-1-phenyl-1-propene (cas 24175-87-9) yield is 800 g.
Step 3. 1-Phenyl-2-propanone (P2P; cas 103-79-7).
1. 2-Acetoxy-1-phenyl-1-propene (cas 24175-87-9) 800 g from Step 2 and sodium hydroxide (NaOH) 600 g in distilled water 2500 ml is stirred at 50 °C for 12 h in 10 L flask with reflux condenser.
2. Reaction solution is extracted with chloroform 1000 ml, dried over magnesium sulphate (Na2SO4) and the solvent is evaporated under vacuum. 1-Phenyl-2-propanone yield is 650 g.
2. Reaction solution is extracted with chloroform 1000 ml, dried over magnesium sulphate (Na2SO4) and the solvent is evaporated under vacuum. 1-Phenyl-2-propanone yield is 650 g.
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