HRID1195922

反应详情

EQUATION

反应方程式

HRID 1195922 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A N,N-dimethylformamide solution (DMF, 100ml) of 3,4-dichloroaniline (6.48 g, 40 mmol) and ethenesulfonyl fluoride (6.7 g, 57.9 mmol) was warmed to 110° C. for three hours. The cooled dark solution was diluted to 400 ml with water and the resulting dark oily precipate was decanted from the supernatant layer. This layer was extracted with ether (4×50 ml). The combined ether extracts were added to the oily precipitate and this dark solution was washed with brine and dried over MgSO4. The organic solution was evaporated to give the crude 2-[(3,4-dichlorophenyl)amino]ethenesulfonyl fluoride as a dark liquid in quantitative yield.

WORKUP

后处理

  1. customthe resulting dark oily precipate was decanted from the supernatant layer
  2. extractionThis layer was extracted with ether (4×50 ml)
  3. additionThe combined ether extracts were added to the oily precipitate
  4. washthis dark solution was washed with brine
  5. dry with materialdried over MgSO4
  6. customThe organic solution was evaporated