反应详情

温度

70 °C

Oxymorphone free base (5.0027 g) was combined with water (2.5 mL) and 2-propanol (6.0 mL) in a round bottom flask (250 mL). The resulting mixture was heated in a temperature controlled bath, with stirring, from ambient to 60° C. over a time period of approximately 30 minutes. Concentrated hydrochloric acid (1.8 mL) was added with continued stirring. The temperature was increased to 70° C. resulting in a clear solution and then cooled to 60° C. 2-propanol was added in 3-5 mL aliquots over approximately 5 minute time span. Solids were observed after the addition of the second aliquot. The resulting slurry was cooled from 60 to 5° C. over 190 minutes and stirred at 5° C. for 45 minutes. Tan solids in a brown solution were observed. The flask was removed from the bath, the contents were vacuum filtered and the solids rinsed 5 times with 1 mL aliquots of 2-propanol:water (9:1 v:v). The resulting white solids were allowed to air-dry for 2 days to yield Form B oxymorphone HCl.

1. temperatureThe resulting mixture was heated in a temperature
2. customambient to 60° C.
3. customover a time period of approximately 30 minutes
4. customresulting in a clear solution
5. temperaturecooled to 60° C
6. additionafter the addition of the second aliquot
7. temperatureThe resulting slurry was cooled from 60 to 5° C. over 190 minutes
8. stirringstirred at 5° C. for 45 minutes
9. customThe flask was removed from the bath
10. filtrationfiltered
11. washthe solids rinsed 5 times with 1 mL aliquots of 2-propanol:water (9:1 v:v)
12. customto air-dry for 2 days