Hydrochloric Acid → Oxycodone Hydrochloride

Participants

Reaction Conditions

Reaction Steps

To a 10 mL flask is charged 1.0 g (3.17 mmol, Lot 2377-103) of oxycodone base (from Example 7) 3.2 mL ethanol and 0.63 mL of water. The mixture is stirred at room temperature (RT, 20±5° C.). A slurry is resulted. The batch is heated to 45° C., added 0.326 g (3.31 mmol, 1.044 molar equivalents) of 37% hydrochloric acid, and a solution is then resulted. The mixture is heated to 55° C. and stirred at 55° C. for 10 hours. Cooled to RT and then to 0-5° C. The mixture is stirred at 0-5° C. for 1.5 hours, filtered, rinsed with cold ethanol (2 mL×2) and dried. 1.021 g of oxycodone HCl (91.4% yield, as Lot 2377-107) is obtained. (3 ppm 14-hydroxycodeinone, undetected 8α,14-dihydroxy-7,8-dihydrocodeinone by LC/MS, and 8β,14-dihydroxy-7,8-dihydrocodeinone by LC/MS; 99.84A % pure by HPLC).

Provenance & Evidence