HRID729002
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
In an autoclave, under pressure and at room temperature, 17 g of ammonia ispassed into a solution of 19.4 g of benzo-1,2,3-thiadiazole-7-carboxylic acid methyl ester in 70 ml of tetrahydrofuran. The solution is then heatedand maintained at 80°-90° C. for approximately 20 hours, an internal pressure of 55·105Pa max. building up. Partial concentration by evaporation is then carried out and the resulting precipitate is filtered off, washed with cold tetrahydrofuran and dried. 14.9 g of beige crystals having a melting point of 270°-272°C. are obtained.
WORKUP
后处理
- customat room temperature
- temperatureThe solution is then heatedand maintained at 80°-90° C. for approximately 20 hours
- concentrationPartial concentration
- customby evaporation
- filtrationthe resulting precipitate is filtered off
- washwashed with cold tetrahydrofuran
- customdried
- customare obtained