反应详情

温度

40 °C

Nilotinib base (3.85 g, 7.27 mmol) was suspended in TFE (19 ml, 5V) and the mixture was heated to 40° C. with stirring. To the resulting cloudy yellow solution, maleic acid (0.84 g, 7.27 mmol) was added in one portion, followed by TFE (19 ml, 5V) at 45-50° C. Dissolution of the solid was achieved after about 5 min stirring at the same temperature. The resulting clear yellow solution was then stirred at 45° C. for about 3 h, and then at room temperature overnight (about 19 h). MTBE (10V) was added with stirring, leading to immediate precipitation. The resulting slurry was stirred for 1 h at room temperature and then the solid was separated from the mother liquors by filtration. The yellow solid was isolated and dried in a vacuum oven (35 mmHg) at 40° C. for 18.5 h to give Nilotinib maleate form IV (3.49 g, 74%) as a pale yellow solid.

1. dissolutionDissolution of the solid
2. stirringstirring at the same temperature
3. stirringThe resulting clear yellow solution was then stirred at 45° C. for about 3 h
4. customat room temperature
5. customovernight (about 19 h)
6. stirringwith stirring
7. customleading to immediate precipitation
8. stirringThe resulting slurry was stirred for 1 h at room temperature
9. customthe solid was separated from the mother liquors by filtration
10. customThe yellow solid was isolated
11. customdried in a vacuum oven (35 mmHg) at 40° C. for 18.5 h