反应详情

温度

60 °C

A reaction vessel is charged with 50.1 g of oxymorphone base, prepared as in Example 1.2B, together with 120 g of absolute alcohol. The mixture is heated to 60±2° C. and stirred to form a slurry. A hydrochloric acid solution prepared from 32.7 g concentrated hydrochloric acid and 33.6 g of water is added to the oxymorphone base slurry and the pH is checked to ensure that it is <1.0. 2.0 g of 10% Pd on carbon catalyst water-wet paste is added under a stream of nitrogen to the reaction mixture and the mixture is hydrogenated at 35 psi (2.41 bar) for 20 hours whilst maintaining a temperature of 65° C. The reaction mixture is filtered whilst hot through Celite. The filtrate is cooled to 0-5° C. over 2-3 hours, and stirred for a further 2 hours to form oxymorphone hydrochloride as a precipitate. The precipitate is filtered off, washed with absolute alcohol and then dried to afford white crystals in 77% yield.

1. customto form a slurry
2. temperaturewhilst maintaining a temperature of 65° C
3. filtrationThe reaction mixture is filtered whilst hot through Celite
4. temperatureThe filtrate is cooled to 0-5° C. over 2-3 hours
5. stirringstirred for a further 2 hours