反应详情

温度

55 °C

Dissolve 4-{4-[4-(4-fluoro-3-trifluoromethyl-phenyl)-1-methyl-1H-imidazol-2-yl]-piperidin-1-yl}-1H-pyrazolo[3,4-d]pyrimidine (20 g, 44.9 mmoles) in a 20:1 H2O:acetone mixture (360 mL). Add a solution of p-toluenesulfonic acid monohydrate (10.25 g; 53.9 mmoles; 1.2 eq) in a 20:1 H2O: acetone mixture (40 mL) to the reaction over 20 minutes at 20° C. Heat the reaction mixture to 55° C., hold for 1 hour, then cool to 25° C. over 1 hour. Filter the solid and wash the cake with water (40 mL). Drying under vacuum at 50° C. affords 4-{4-[4-(4-fluoro-3-trifluoromethyl-phenyl)-1-methyl-1H-imidazol-2-yl]-piperidin-1-yl}-1H-pyrazolo[3,4-d]pyrimidine p-toluenesulfonate (23.9 g; 86%) as a white solid.

1. temperaturecool to 25° C. over 1 hour
2. filtrationFilter the solid
3. washwash the cake with water (40 mL)
4. customDrying under vacuum at 50° C.