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
4.0 g (29 mmol) of potassium carbonate were added to a solution of 5.0 g (29 mmol) of 2-hydroxybenzenesulfonamide in 200 ml of acetonitrile at 25° C. Stirring was carried out for 10 minutes, after which 4.1 g (29 mmol) of dimethylaminosulfonyl chloride were added dropwise at 25° C. and stirring was continued for a further 16 hours at this temperature. The volatile constituents were removed under reduced pressure from a water pump, the residue was taken up in ethyl acetate, the solution was dried over Na2SO4 and the solvent was removed under reduced pressure from a water pump. The remaining residue was stirred vigorously for 1 hour with 100 ml of diethyl ether. The crystalline product was filtered off under suction and dried at 40° C. under reduced pressure. 5.7 g of the title compound were obtained in this manner.
WORKUP
后处理
- stirringstirring
- waitwas continued for a further 16 hours at this temperature
- customThe volatile constituents were removed under reduced pressure from a water pump
- dry with materialthe solution was dried over Na2SO4
- customthe solvent was removed under reduced pressure from a water pump
- stirringThe remaining residue was stirred vigorously for 1 hour with 100 ml of diethyl ether
- filtrationThe crystalline product was filtered off under suction
- customdried at 40° C. under reduced pressure