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 N,N-dimethylacetamide (10 mL). The clear solution was stirred at 23 to 25° C. (24 hours) and the resulting white suspension was filtered, washed with ethyl acetate (2×5 mL) and air-dried for 16 hours to yield 655 mg of tofacitinib hydrochloride as a white solid. 1H NMR analysis showed a molar ratio of tofacitinib hydrochloride to N,N-dimethylacetamide of approximately 1:0.9 (18.3 wt %). A PXRD taken of this sample is shown in FIG. 8.

1. filtrationthe resulting white suspension was filtered
2. washwashed with ethyl acetate (2×5 mL)
3. customair-dried for 16 hours