HRID1373121

反应详情

EQUATION

反应方程式

HRID 1373121 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6.8 g (29.8 mmol) of N-(2-dimethylamino-ethyl)-phenylsulphonamide are dissolved in 100 ml of DMF and combined with 1.3 g (30 mmol) of sodium hydride (55% in oil). The mixture is stirred for one hour at ambient temperature. Then 4.2 g (29.8 mmol) of 4-fluoro-nitrobenzene are added, and stirring is continued for another 16 hours. After the addition of 300 ml of water the mixture is extracted with ethyl acetate. The organic phase is washed with water, dried and evaporated down. The residue is acidified with 1 N hydrochloric acid and washed with ethyl acetate. The aqueous phase is then made basic again with sodium hydroxide solution and extracted with ethyl acetate. The organic phase is dried and evaporated down.

WORKUP

后处理

  1. stirringstirring
  2. waitis continued for another 16 hours
  3. extractionis extracted with ethyl acetate
  4. washThe organic phase is washed with water
  5. customdried
  6. customevaporated down
  7. washwashed with ethyl acetate
  8. extractionextracted with ethyl acetate
  9. customThe organic phase is dried
  10. customevaporated down