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 acetonitrile (10 mL). A gummy suspension was formed, which was stirred for 26 hours at 23 to 25° C. The resulting white suspension was filtered, washed with acetonitrile (2×5 mL) and air-dried to yield 570 mg of tofacitinib hydrochloride as a white solid. 1H NMR analysis showed a molar ratio of tofacitinib hydrochloride to acetonitrile of approximately 1:0.08 (0.9 wt %). A PXRD taken of this sample is shown in FIG. 7. A sample was further dried at 58° C. at 40 torr for 24 hours. 1H NMR analysis showed a molar ratio of tofacitinib hydrochloride to acetonitrile of approximately 1:0.01 (0.1 wt %). Water content (KF) was 0.57%. The PXRD remained the same as shown in FIG. 7.

1. customA gummy suspension was formed
2. filtrationThe resulting white suspension was filtered
3. washwashed with acetonitrile (2×5 mL)
4. customair-dried