反应详情

温度

24 °C

A solution of 4M hydrogen chloride in 1,4-dioxane (2.353 mmol) was added to a suspension of tofacitinib free base (0.7 g, 2.24 mmol) in methyl ethyl ketone (10 mL). The resulting white suspension was stirred for 25 hours at 23 to 25° C., filtered, washed with methyl ethyl ketone (2×5 mL) and air-dried for 16 hours to yield 760 mg of tofacitinib hydrochloride as a white solid. 1H NMR analysis showed a molar ratio of tofacitinib hydrochloride to methyl ethyl ketone of approximately 1:0.52 (9.7 wt %). A PXRD taken of this sample is shown in FIG. 10.

1. filtrationfiltered
2. washwashed with methyl ethyl ketone (2×5 mL)
3. customair-dried for 16 hours