反应详情

温度

65 °C

4-Methyl-N-[3-(4-methyl-imidazol-1-yl)-5-trifluoromethyl-phenyl]-3-(4-pyridin-3-yl-pyrimidin-2-ylamino)-benzamide hydrochloride (12 g) is suspended in 192 mL of methanol and 14.87 mL of water. The solution is heated to 64-66° C. in 10 minutes and kept for minutes at 66° C. The solution is then cooled down to 42° C. in 15 minutes and then seeded. The suspension is kept for 2.5 hours at 42° C. and cooled down to 20° C. in 7 hours and cooled down within 6 hours at −10° C. The suspension is kept for 79 hours before filtration under vacuum. The solid is washed 2 times with a cold mixture of methanol/water 66 mL/5.26 mL (−10° C.) and dried under vacuum at 70° C. for 20 hours to obtain form C 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.

1. waitkept for minutes at 66° C
2. temperatureThe solution is then cooled down to 42° C. in 15 minutes
3. temperaturecooled down to 20° C. in 7 hours
4. temperaturecooled down within 6 hours at −10° C
5. filtrationThe suspension is kept for 79 hours before filtration under vacuum
6. washThe solid is washed 2 times
7. additionwith a cold mixture of methanol/water 66 mL/5.26 mL (−10° C.)
8. customdried under vacuum at 70° C. for 20 hours