反应详情

温度

55 °C

A reaction vessel is charged with 2.5 g of oxymorphone base, prepared as in Example 2.2B, together with 7.5 mL of absolute alcohol, 2.5 g of water and 1.66 g of concentrated hydrochloric acid. The mixture is heated to 50-60° C. and a solution results. The pH is checked to ensure that it is <1.0. 0.111 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±5 psi (2.41 bar) for 21 hours whilst maintaining a temperature of 65±3° C. The reaction mixture is filtered whilst hot through a 0.45 μm filter. 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 cold absolute alcohol and dried under vacuum to afford white crystals in 77% yield.

1. customa solution results
2. temperaturewhilst maintaining a temperature of 65±3° C
3. filtrationThe reaction mixture is filtered whilst hot through a 0.45 μm
4. filtrationfilter
5. temperatureThe filtrate is cooled to 0-5° C. over 2-3 hours