反应详情

温度

24 °C

A solution of 4M hydrogen chloride in 1,4-dioxane (6.722 mmol) was added to a suspension of tofacitinib free base (2.0 g, 6.402 mmol) in acetone (25 mL). The suspension was stirred at 23 to 25° C. for 16 hours, filtered and washed with acetone (2×10 mL) to yield a damp cake (5.15 g) of tofacitinib hydrochloride as a white solid. A PXRD taken of the damp cake is shown in FIG. 1. A sample was air-dried over 3 days and 2.3 g of this dried material was suspended in refluxing acetone (30 mL) for 24 hours. The suspension was cooled to 23 to 25° C., filtered, washed with acetone (2×5 mL) and air-dried for 16 hours to yield tofacitinib hydrochloride (2.24 g) as a white solid. 1H NMR analysis showed a molar ratio of tofacitinib hydrochloride to acetone of approximately 1:0.86 (12.5 wt %). Water content (KF) was 0.0%. A PXRD taken of this sample is shown in FIG. 2.

1. filtrationfiltered
2. washwashed with acetone (2×10 mL)