反应详情

温度

5 °C

Nilotinib base (0.300 g, 0.57 mmol) was dissolved in TFE (2 mL) at 40° C. to obtain a mixture. The mixture was stirred and added to a solution of 2-chloromandelic acid (0.106 g, 0.57 mmol) in TFE (1 mL) at 40° C. Stirring of the resulting clear solution was continued for about 4 h at 40° C. and the solution was subsequently cooled to 5° C. The mixture was kept at 5° C. overnight and then methyl tert-butyl ether (MTBE) (1.5 v/v) was added to the mixture at room temperature, leading to precipitation. The precipitate was filtered to give a white solid of Nilotinib 2-chloromandelate form I.

1. customto obtain a mixture
2. stirringStirring of the resulting clear solution
3. waitThe mixture was kept at 5° C. overnight
4. customleading to precipitation
5. filtrationThe precipitate was filtered