反应详情

温度

50 °C

Acetone (845 uL) was added to the crystalline 3-[2-{[3-(diethylamino)propyl]-amino}-8-(2,6-difluorophenyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide-free-base (46.9 mg), and the resulting mixture was heated to 50° C. Phosphoric acid was added (1.0 equivalents; 1M in methanol). Additional methanol (5 uL) was added to the resulting oily mixture to increase solubility slightly. The mixture was cooled to room temperature and stirred overnight. The product was filtered and dried for at least one hour in a vacuum oven at 50° C. with a slow nitrogen bleed. The yield was 67.1% (36.9 mg) of partially crystalline 3-[2-{[3-(diethylamino)propyl]amino}-8-(2,6-difluorophenyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide phosphate salt.

1. temperatureto increase solubility slightly
2. temperatureThe mixture was cooled to room temperature
3. filtrationThe product was filtered
4. customdried for at least one hour in a vacuum oven at 50° C. with a slow nitrogen