Hydrochloric Acid → Oxycodone Hydrochloride

Participants

Reaction Conditions

Reaction Steps

An aqueous solution of HCl (87.0 kg of water and 13.00 kg of conc. HCl) is stirred with 48 kg of Oxycodone base at 80° C., activated carbon and diatomaceous earth are added and, after stirring for 15 min, the suspension is filtered, the filtrate is gradually cooled down to the final temperature of 1 to 3° C. Precipitated crystals are centrifuged off, washed with ethanol, and Oxycodone hydrochloride is dried at temperature of about 70 to 80° C. 51.2 kg of (91%) Oxycodone hydrochloride is obtained, m.p. 219° C, [α]D2°—145°, water content 6.0%, purity 99.4% (RP C8 column, 150×3.9 mm, 5 μm, with a RP C8 pre-column, 20×3.9 mm, 5 μm, mobile phase 0.005 mol/l sodium hexane sulfonate-methanol-phosphoric acid-triethyl-amine (v/v) (900:100:5:2), pH=2.5 adjusted with NaOH; flow rate 1.5 ml/min; temperature 50° C.; UV, λ=206 run), content 100.03% (titration).

Provenance & Evidence