HRID1720848

反应详情

EQUATION

反应方程式

HRID 1720848 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Chlorobenzoyl cyanide (13.0 g, 0.079 mol) prepared in Example 1a was added to a stirred mixture of sodium bromide (1.0 g, 0.01 mol) and 80% sulphuric acid (10 ml). An exothermic reaction took place with the formation of a solid yellow mass. Ethanol (50 ml) was added and the mixture was heated under reflux to give a yellow solution. On cooling, a colourless precipitate formed. The mixture was diluted with cold water and extracted with isopropyl ether. The organic extract was washed with water, sodium bicarbonate solution and then again with water and dried over sodium sulphate. Evaporation and distillation of the solution gave the product as a yellow oil (8.2 g, 54%)--b.p. 82°-84° C./0.05 mm Hg.

WORKUP

后处理

  1. customAn exothermic reaction
  2. temperaturethe mixture was heated
  3. temperatureunder reflux
  4. customto give a yellow solution
  5. temperatureOn cooling
  6. customa colourless precipitate formed
  7. extractionextracted with isopropyl ether
  8. extractionThe organic extract
  9. washwas washed with water, sodium bicarbonate solution
  10. dry with materialagain with water and dried over sodium sulphate
  11. customEvaporation and distillation of the solution