Formic Acid → Oxycodone

Participants

Reaction Conditions

Reaction Steps

50 kg thebaine was added to a solution of formic acid (145 kg) maintained at a temperature below 15° C. the solution was heated to 25° C. and maintained at this temperature for 1.0 hr. the reaction mixture was cooled to 0-5° C. and 30% H2O2 aqueous solution (5.5 kg 100% H2O2) was added at 0-5° C. The reaction mixture was maintained at 20-25° C. for 3.0 hrs. After completion of the reaction, it was quenched in 560 lit DM water and treated with charcoal. To the filtrate 5% Pd/C (1.5 kg) was added and hydrogen gas purged at 20-25° C. The reaction mixture was maintained at 20-25° C. for 4-5 hrs. After reaction completion, the catalyst was filtered off and the pH of the filtrate was adjusted to 9-9.5 with aqueous ammonia. The product was extracted with methylene dichloride and subsequently concentrated to obtain a solid which was isolated with IPA. Yield: 41.7 kg

Provenance & Evidence