HRID1647662

反应详情

EQUATION

反应方程式

HRID 1647662 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringstirring
  2. waitwas continued for a further 16 hours at this temperature
  3. customThe volatile constituents were removed under reduced pressure from a water pump
  4. dry with materialthe solution was dried over Na2SO4
  5. customthe solvent was removed under reduced pressure from a water pump
  6. stirringThe remaining residue was stirred vigorously for 1 hour with 100 ml of diethyl ether
  7. filtrationThe crystalline product was filtered off under suction
  8. customdried at 40° C. under reduced pressure