反应详情

温度

40 °C

A slurry of benzoic acid (3.95 kg, 32.33 mol) and (4-chloro-7-(3-cyanophenyl)isoquinolin-1-yl)guanidine (10.2 kg, 31.69 mol) in DMA (61.2 L) was heated at 60° C. until dissolution was complete. The solution was slowly cooled to 40° C., seeded, granulated at 40° C. and then at ambient temperature. The thick slurry was cooled to 0° C., granulated, and the solid was collected by filtration, washed with DMA (5.1 L) and MeCN (10.2 L) and dried overnight in vacuo at 55° C to give (4-chloro-7-(3-cyanophenyl)isoquinolin-1-yl)guanidinium benzoate (9.85 kg, 22.19 mol, 70%) as an off white solid.

1. customgranulated at 40° C.
2. customat ambient temperature
3. temperatureThe thick slurry was cooled to 0° C.
4. filtrationthe solid was collected by filtration
5. washwashed with DMA (5.1 L) and MeCN (10.2 L)
6. customdried overnight in vacuo at 55° C