反应详情

温度

130 °C

A stirred suspension of guanidine carbonate (720 g, 4.0 mol) in NMP (5 L) was heated to 130° C. under N2 for 1 hour. The suspension was cooled to room temperature and 1,4-dichloro-7-(3-cyanophenyl)isoquinoline (1.0 kg, 3.3 mmol) was added as a solid. The mixture was heated at 130° C. for 4 hours, cooled to room temperature, filtered through a pad of clarcel. Water (6.7 L) was added to the filtrate. The resultant slurry was cooled to 5° C., stirred for 1 hour and the solid collected by filtration. The solid was washed with a mixture of NMP:water (1:1, 4 L) and water (4 L) and dried in vacuo at 50° C. to give (4-chloro-7-(3-cyanophenyl)isoquinolin-1-yl)guanidine (900 g, 2.8 mol, 85%) as a green solid.

1. temperatureThe suspension was cooled to room temperature
2. temperatureThe mixture was heated at 130° C. for 4 hours
3. temperaturecooled to room temperature
4. filtrationfiltered through a pad of clarcel
5. additionWater (6.7 L) was added to the filtrate
6. temperatureThe resultant slurry was cooled to 5° C.
7. filtrationthe solid collected by filtration
8. washThe solid was washed with a mixture of NMP:water (1:1, 4 L) and water (4 L)
9. customdried in vacuo at 50° C.