Hydrochloric Acid → HCID 131734729, compound

Participants

Reaction Steps

A solution of 4M hydrogen chloride in 1,4-dioxane (0.6 mL, 2.353 mmol) was added to a solution of tofacitinib free base (0.7 g, 2.24 mmol) in nitromethane (6 mL). Gummy solids were obtained when ethyl acetate (6 mL) was added. Stirring was continued at 23 to 25° C. for 23 hours and the resulting white suspension was filtered, washed with ethyl acetate (2×5 mL) and air-dried to yield 800 mg of tofacitinib hydrochloride as a white solid. 1H NMR analysis showed a molar ratio of tofacitinib hydrochloride to nitromethane of approximately 1:0.009 (0.1 wt %). A PXRD taken of this sample is shown in FIG. 11.

Provenance & Evidence