反应详情

温度

65 °C

36.0 g 4-methyl-N-[3-(4-methyl-imidazol-1-yl)-5-trifluoromethyl-phenyl]-3-(4-pyridin-3-yl-pyrimidin-2-ylamino)-benzamide hydrochloride is dissolved in a solvent mixture of 576 mL of methanol and 44.61 mL of water at 52° C. The solution is heated up to 64-66° C. in 15 minutes and kept for 5 minutes at 66° C. Then the solution is cooled down at 42° C. in minutes and the solution is seeded. The suspension is kept for 2.5 hours at 42° C., cooled down within 7 hours at 20° C., and maintained at this temperature for 11 hours. The methanol solvate form SC of the hydrochloride salt of 4-methyl-N-[3-(4-methyl-imidazol-1-yl)-5-trifluoromethyl-phenyl]-3-(4-pyridin-3-yl-pyrimidin-2-ylamino)-benzamide is obtained.

1. temperatureThen the solution is cooled down at 42° C. in minutes
2. waitThe suspension is kept for 2.5 hours at 42° C.
3. temperaturecooled down within 7 hours at 20° C.
4. temperaturemaintained at this temperature for 11 hours