反应详情

温度

20 °C

Into a 5 L reactor equipped with an overhead stirrer and reflux condenser was dissolved N,N-dimethyl barbituric acid (32.56 g, 208.5 mmol) and tetrakis(triphenylphosphine)palladium[0](20.36 g, 17.6 mmol) in dichloromethane (1.5 L). The mixture was stirred at a temperature of about 20° C. Into the mixture was charged naloxone (110.90 g, 338.8 mmol) as a suspension in dichloromethane (1 L). The resulting reaction mixture was stirred at 38° C. for 16 hours. The mixture was cooled to a temperature of about 20° C. and the solids were filtered off under reduced pressure. The solids were washed with dichloromethane (5 L) followed by washing with water (2.5 L). The solids were dissolved into a 10:1 mixture of water:concentrated sulfuric acid at 40° C. The heated aqueous solution was washed with dichloromethane (0.5 L) and then basified to a pH of 9.05 with 28% ammonium hydroxide. The resulting solids were filtered and dried under reduced pressure at 100° C. for 20 hours to provide noroxymorphone as a white solid (87.12 g, 303.2 mmol).

1. customInto a 5 L reactor equipped with an overhead stirrer
2. temperaturereflux condenser
3. customThe resulting reaction mixture
4. stirringwas stirred at 38° C. for 16 hours
5. temperatureThe mixture was cooled to a temperature of about 20° C.
6. filtrationthe solids were filtered off under reduced pressure
7. washThe solids were washed with dichloromethane (5 L)
8. washby washing with water (2.5 L)
9. dissolutionThe solids were dissolved into a 10:1 mixture of water
10. customat 40° C
11. washThe heated aqueous solution was washed with dichloromethane (0.5 L)
12. filtrationThe resulting solids were filtered
13. customdried under reduced pressure at 100° C. for 20 hours