反应详情

As described above, oxycodone base purified (Lot P, 13.56 g, 43.0 mmol) was dissolved (in 80-mL beaker over 15 minutes) in the mixture of water (13 mL) and acetic acid (3.0 mL) at ambient temperature. Hydrochloric acid (10.41 mol/kg, 5.0 g or 51.6 mmol) was added to the solution over 5 minutes. Stirring was continued for another 40 minutes and IPA (55 mL) was added over 15 minutes. Stirring was continued for another 30 minutes. Precipitated product was filtered off, washed on filter with IPA (2×20 ml) and acetone (2×20 mL), dried on filter providing 14.74 g oxycodone HCl (39.86 mmol or 93% yield on OC base purified)—lot Q.

1. custompurified (Lot P, 13.56 g, 43.0 mmol)
2. dissolutionwas dissolved (in 80-mL beaker over 15 minutes)
3. additionin the mixture of water (13 mL) and acetic acid (3.0 mL) at ambient temperature
4. stirringStirring
5. waitwas continued for another 30 minutes
6. filtrationPrecipitated product was filtered off
7. washwashed
8. filtrationon filter with IPA (2×20 ml) and acetone (2×20 mL)
9. customdried
10. filtrationon filter