Water → Oxymorphone

Participants

Reaction Steps

Oxycodone (10.0 g) was suspended in chloroform (CHCl3, 150 mL) in a reactor A. Boron tribromide (BBr3, 10.0 mL) was added slowly and an exotherm was observed. The reaction temperature was maintained below 25° C. during the addition. Stirring of the mixture was continued at room temperature for 14 hours. The material was transferred to reactor B that was pre-filled with 85 mL of water. The temperature reached 50 to 55° C. and was maintained below 55° C. during the addition. After transfer of the mixture to reactor B, some solid residue still remained in reactor A. The mixture in reactor B was stirred at 50 to 55° C. to dissolve the solid (about 15 minutes) and then when stirring was stopped, the mixture separated into two clear layers. The aqueous solution in reactor B was transferred back to reactor A. The mixture was stirred at 50 to 55° C. for 15 to 30 minutes to dissolve all the solids. The organic layer in reactor B was extracted with H3PO4/H2O solution (2% wt/wt, 15 mL). The aqueous extraction was transferred to reactor A. The solution in reactor A was extracted with dichloroethane (30 mL) and then allowed to separate into two phases.

Provenance & Evidence