反应详情

温度

25 °C

19.6 g of a solution of 6.1 g of 5-chloro-2-(i-propoxycarbonyl)benzenesulfonyl isocyanate (20 mmol) in 1,2-dichloroethane are added dropwise to a solution of 3.9 g of 2-amino-4-methoxy-6-trifluoromethyl-1, 3,5-triazine (20 mmol) in 150 ml of 1,2-dichloroethane at 25° C. The mixture is stirred at 25° C. for 16 h and then at 50° C. for 3 h. After removal of volatiles under waterpump vacuum at 60° C., the residue is extracted with 200 ml of a mixture of tert-butyl methyl ether and diethyl ether. The solvents are removed under waterpump vacuum at 50° C. and the residue is stirred in a little i-propanol. The solid product is filtered off with suction and dried under waterpump vacuum at 40° C. This results in 7.2 g of the title compound (14 mmol; 70% of theory) of melting point 160°-163° C.

1. waitat 50° C. for 3 h
2. customAfter removal of volatiles under waterpump vacuum at 60° C.
3. extractionthe residue is extracted with 200 ml of a mixture of tert-butyl methyl ether and diethyl ether
4. customThe solvents are removed under waterpump vacuum at 50° C.
5. stirringthe residue is stirred in a little i-propanol
6. filtrationThe solid product is filtered off with suction
7. customdried under waterpump vacuum at 40° C