反应详情

温度

55 °C

A suspension of tofacitinib free base (1.0 g, 3.201 mmol) in isopropanol was heated to 55° C. to dissolve. A solution of approximately 17 wt % hydrogen chloride in isopropanol (825 mg, 3.84 mmol) was added. The solution was then cooled to 23 to 25° C. whereupon slightly gummy solids precipitated out. The suspension was stirred at 23 to 25° C. for 64 hours, filtered and washed with isopropanol (2×12 mL). The damp cake was dried under vacuum (45 torr) at 40° C. (24 hours) to yield amorphous tofacitinib hydrochloride (612 mg).

1. dissolutionto dissolve
2. temperatureThe solution was then cooled to 23 to 25° C. whereupon slightly gummy solids
3. customprecipitated out
4. filtrationfiltered
5. washwashed with isopropanol (2×12 mL)
6. customThe damp cake was dried under vacuum (45 torr) at 40° C. (24 hours)