反应详情

温度

81 °C

Morphine sulfate (30.0 g), water (30 mL), and EtOH (60 mL) were added to a reaction flask. 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 reaction flask was charged with the catalyst (RuCl3.xH2O, 0.60 g), and the mixture was heated to reflux (80-82° C.) for 16 h. HPLC analysis indicated that 94.5% (area) hydromorphone was formed. Acetonitrile (30 mL) was added to the reaction mixture and the mixture was heated for 1 h. EtOH (90 mL) was added to the mixture, which was then cooled to 15° C. for 2 h. The mixture was filtered, and the solid was washed with 95% EtOH (2×15 mL). The solid was dried under vacuum at 65° C. for 18 h to give 13.8 g of hydromorphone sulfate as solids (purity>99% 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 mixture was heated
5. customwas formed
6. temperaturethe mixture was heated for 1 h
7. temperaturewas then cooled to 15° C. for 2 h
8. filtrationThe mixture was filtered
9. washthe solid was washed with 95% EtOH (2×15 mL)
10. customThe solid was dried under vacuum at 65° C. for 18 h