HRID358640

反应详情

EQUATION

反应方程式

HRID 358640 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of methyl 10-bromodecanoate (1.5 g, 0.006 mol), 4-chlorobenzenesulphonamide (3.44 g, 0.018 mol), potassium carbonate (6.2 g, 0.045 mol) and dimethylformamide (50 ml) was heated at 100°-120° C. for 3 hours. After cooling, the inorganic material was removed by filtration. The filtrate was evaporated to dryness and the residue was extracted with dichloromethane. The residual oil obtained by evaporation was chromatographed on silica gel in petroleum ether (40°-60° C.) and the solid obtained on evaporation of the eluate was recrystallised (ether-pet. ether 40°-60°) to give the title compound (0.9 g, m.p. 68°-70° C.).

WORKUP

后处理

  1. temperaturewas heated at 100°-120° C. for 3 hours
  2. temperatureAfter cooling
  3. customthe inorganic material was removed by filtration
  4. customThe filtrate was evaporated to dryness
  5. extractionthe residue was extracted with dichloromethane
  6. customThe residual oil obtained by evaporation
  7. customwas chromatographed on silica gel in petroleum ether (40°-60° C.)
  8. customthe solid obtained on evaporation of the eluate
  9. customwas recrystallised (ether-pet. ether 40°-60°)