Water → HCID 46781713, compound

Participants

Reaction Conditions

Reaction Steps

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).

Provenance & Evidence