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Synthesis of P2P from P2NP with NaBH4 via K2CO3/H2O2 system (1kg scale)

William Dampier

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Synthesis:
1. 1000 g 1-phenyl-2-nitropropene was dissolved in 10000 ml methanol.
2. The reaction mixture was cooled to 0 *C with an ice/salt bath with good stirring.
3. 470 g NaBH4 were added in small portions, so that the temperature was not allowed to rise above 15 *С.
4. After stop exothermic reaction, the ice/salt-bath was removed.
5. The solution was stirred at room temperature for two hours.
6. After this time, the solution was cooled to 0 *C in ice/salt-bath again.
7. Added 6000 ml 30% H2O2 with 1800 g K2CO3 in flask.
8. The solution was left to stir for 24 hours at room temp.
9. After this time, dropwise aqueous HCl in solution at pH < 7 (exothermic reaction, CO2 discharge).
10. Extracted with 5000 ml CH2CI2, washed with 5000 ml 25% aqua. NaOH and 5000 ml H2O.
11. The CH2Cl2 removed under vacuum to give a clear yellow oil, yield 70%.
 
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