反应详情

温度

81 °C

A reaction flask was charged with morphine sulfate (40.0 g), water (30 mL), and EtOH (60 mL). The reaction mixture was agitated to form a suspension. The reactor was flushed with nitrogen and the reaction mixture was kept under nitrogen throughout the reaction. The flask was charged with acetone (0.4 mL) and the catalyst (RuCl3.xH2O, 0.60 g). The reaction mixture was heated to reflux (80-82° C.) and maintained at that temperature for 24 h. HPLC analysis indicated that 93% (area) hydromorphone was formed. Acetonitrile (6 mL) was added to the reaction mixture and the mixture was heater under reflux for 2 h. EtOH (180 mL) was added to the mixture, which was then cooled down to 10° C. for 2 h. The mixture was filtered, and the solid was washed with 95% EtOH (3×15 mL). The solid was dried at 90° C. for 28 h to give 32.2 g of hydromorphone sulfate as solids (purity>98% area).

1. customto form a suspension
2. customThe reactor was flushed with nitrogen
3. customthe reaction mixture was kept under nitrogen throughout the reaction
4. temperatureThe reaction mixture was heated
5. temperaturemaintained at that temperature for 24 h
6. customwas formed
7. temperatureunder reflux for 2 h
8. temperaturewas then cooled down to 10° C. for 2 h
9. filtrationThe mixture was filtered
10. washthe solid was washed with 95% EtOH (3×15 mL)
11. customThe solid was dried at 90° C. for 28 h