反应详情

温度

20 °C

To a 1 Liter reactor was added Nilotinib-base form A (20 g, 0.04 mol), absolute ethanol (200 ml), and HCl 32% solution in water (6.45 g, 0.04 mol). A slurry was formed. The slurry was heated to reflux, dissolution occurred during the stirring, and the solution was then filtered under reduced pressure. The filtrate was fed to a second reactor and heated back to reflux. At 76.0° C. the solution was seeded with 0.2 g of a dry material obtained by the process of example 23. Precipitation was observed. Then, the mixture was maintained at reflux for 0.5 h, followed by cooling over 2 h to 5° C. During cooling at 20° C. absolute ethanol was added (100 ml) and the slurry was stirred till it cooled to 5° C. The cooled slurry was then filtered, and the collected solid was washed with absolute ethanol, and dried over night at 70° C. in a vacuum oven to yield Nilotinib-HCl form T17 (16.3 g, 73% yield).

1. customA slurry was formed
2. temperatureThe slurry was heated
3. temperatureto reflux
4. dissolutiondissolution
5. filtrationthe solution was then filtered under reduced pressure
6. customThe filtrate was fed to a second reactor
7. temperatureheated back
8. temperatureto reflux
9. customAt 76.0° C.
10. customobtained by the process of example 23
11. customPrecipitation
12. temperatureThen, the mixture was maintained
13. temperatureat reflux for 0.5 h
14. temperatureby cooling over 2 h to 5° C
15. additionwas added (100 ml)
16. temperaturecooled to 5° C
17. filtrationThe cooled slurry was then filtered
18. washthe collected solid was washed with absolute ethanol
19. customdried over night at 70° C. in a vacuum oven