反应详情

Oxycodone acetate solution was diluted with isopropanol (25 mL), cooled to ˜10° C. and neutralized at 10° C. to 5° C. with ammonium hydroxide (conc., ˜30 mL until pH ˜9.5). Stirring continued for 10 minutes and precipitated solids were filtered off, washed on filter with water (20 mL, 2×50 mL, 10 mL) and dried on filter for 0.5 hours. The light gray wet material (22.29 g) was prepared. This material was dissolved in chloroform (150 mL), treated with sodium sulfate (anhydrous) for one hour. Solvent was removed in vacuum and gray powder was dried on rotary evaporator for one hour at 50° C. in the bath, providing oxycodone base (16.31 g, 51.72 mmol, 74.1% yield on ABUK sulfate). Impurity profile is shown in Table 8.

1. customprecipitated solids
2. filtrationwere filtered off
3. washwashed
4. filtrationon filter with water (20 mL, 2×50 mL, 10 mL)
5. customdried
6. filtrationon filter for 0.5 hours
7. customSolvent was removed in vacuum and gray powder
8. customwas dried on rotary evaporator for one hour at 50° C. in the bath