反应详情

Under protective gas, a 14.5% strength solution (1465 g) of methyl 4-iodo-2-isocyanatosulfonylbenzoate in xylene is added over 4 hours at a constant rate at 50° C. to a suspension of 84.5 g of 2-amino-4-methoxy-6-methyl-1,3,5-triazine in 670 g of ethyl acetate. After the addition has ended, the mixture is stirred at the same temperature for approximately 4 hours, and the ethyl acetate is then distilled off under reduced pressure (80–60 mbar, T=50° C.). The suspension that remains is filtered off with suction and the solid is washed repeatedly with dilute hydrochloric acid and dried; if appropriate, acetone can be added to the hydrochloric acid. This gives 297 g (content>98%) of the title compound; yield 99.2% of theory.

1. additionAfter the addition
2. distillationthe ethyl acetate is then distilled off under reduced pressure (80–60 mbar, T=50° C.)
3. filtrationThe suspension that remains is filtered off with suction
4. washthe solid is washed repeatedly with dilute hydrochloric acid
5. customdried
6. additionif appropriate, acetone can be added to the hydrochloric acid