Sulfuric Acid → HCID 46781713, compound

Participants

Reaction Conditions

Reaction Steps

A reaction flask was charged with morphine base (30.0 g, wet, 75% wt, 78.85 mmol), water (23 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 reaction flask was charged with H2SO4 (98%, 7.73 g, 78.85 mmol) and the catalysts (RuCl3.xH2O, 0.20 g). The reaction mixture was heated to reflux (80-82° C.) for 24 h. HPLC analysis indicated that 93% (area) hydromorphone was formed. The reaction mixture was cooled down overnight. DMSO (1.0 mL) was added to the reaction mixture and the mixture was heated at reflux for 1 h. The pH of the reaction mixture was adjusted the pH to 1.6 with 50% NaOH. EtOH (90 mL) was added to the mixture, which as cooled down to 15° C. for 1 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 11.8 g of hydromorphone sulfate as solids (purity>99% area).

Provenance & Evidence