GhostChemist
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Phenylacetone (P2P) synthesis
Phenylacetone (P2P) synthesis from P2NP.
https://bbgate.com/threads/p2p-synthesis-from-p2np.188/
https://bbgate.com/threads/p2p-synthesis-from-p2np.188/
- 1-Phenyl-2-nitropropene (P2NP; cas 705-60-2) 1000 g;
- Methanol (MeOH) 10 L;
- Sodium borohydride (NaBH4) 470 g;
- Hydrogen peroxide (H2O2) 30% 6 L;
- Potassium carbonate (K2CO3) 1800 g;
- Hydrochloric acid (HCl) 37% aq;
- Dichloromethane (CH2CI2) 5 L;
- Sodium hydroxide (NaOH) 5 L 25% aq;
- Distilled water (H2O) 5 L;
- 20 L Round bottom flask;
- Water bath, ice;
- HCl gas source;
- Magnetic or top stirrer;
- Retort stand and clamp for securing apparatus;
- Vacuum source;
- Glass rod and spatula;
- Rotovap machine;
- 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;
Reaction scheme:
1. 1-Phenyl-2-nitropropene 1000 g is dissolved by methanol (MeOH) 10 L in 20 L flask.
2. The reaction mixture is cooled to 0 °C by an ice/salt bath with good stirring.
3. Sodium borohydride (NaBH4) 470 g is added to reaction mixture in small portions with a constant stirring in order to control reaction temperature below 15 °C.
4. The ice/salt bath is removed after an exothermic reaction end.
5. The solution is stirred at room temperature for 2 h.
6. Then, the solution is cooled to 0 °C in ice/salt bath again.
7. Hydrogen peroxide (H2O2) 30% 6 L and potassium carbonate (K2CO3) 1800 g are added into the reaction flask.
8. The solution is stirred for 24 h at room temperature.
9. Next, hydrochloric acid (HCl) 37% aq is poured into the mixture dropwise to reach pH 6.5-7. The reaction is exothermic, CO2 is released (caution!).
10. The mixture is extracted with dichloromethane (CH2CI2) 5 L, extract is washed with sodium hydroxide (NaOH) 5 L 25% aq. and distilled water (H2O) 5 L.
11. Dichloromethane (CH2CI2) is distilled off under vacuum to give a clear phenylacetone (P2P, cas 103-79-7) yellow oil. The yield is 70%.
2. The reaction mixture is cooled to 0 °C by an ice/salt bath with good stirring.
3. Sodium borohydride (NaBH4) 470 g is added to reaction mixture in small portions with a constant stirring in order to control reaction temperature below 15 °C.
4. The ice/salt bath is removed after an exothermic reaction end.
5. The solution is stirred at room temperature for 2 h.
6. Then, the solution is cooled to 0 °C in ice/salt bath again.
7. Hydrogen peroxide (H2O2) 30% 6 L and potassium carbonate (K2CO3) 1800 g are added into the reaction flask.
8. The solution is stirred for 24 h at room temperature.
9. Next, hydrochloric acid (HCl) 37% aq is poured into the mixture dropwise to reach pH 6.5-7. The reaction is exothermic, CO2 is released (caution!).
10. The mixture is extracted with dichloromethane (CH2CI2) 5 L, extract is washed with sodium hydroxide (NaOH) 5 L 25% aq. and distilled water (H2O) 5 L.
11. Dichloromethane (CH2CI2) is distilled off under vacuum to give a clear phenylacetone (P2P, cas 103-79-7) yellow oil. The yield is 70%.
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