HRID279142

反应详情

EQUATION

反应方程式

HRID 279142 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
2 °C

PROCEDURE

实验过程

A solution of cyclohexanecarbonyl chloride (9.1 ml) in CH2Cl2 (25 ml) was added slowly under nitrogen atmosphere at 0-4° C. to a stirred mixture of AlCl3 (9.1 g), CH2Cl2 (25 ml) and benzene (50 ml). The resulting mixture was stirred for 1 hour at 0-4° C. and 12 hours at the room temperature. The mixture was poured into ice-water (200 ml, contains 1 ml of concentrated HCl) and stirred for 5 minutes. The phases were separated and the aqueous phase was washed with CH2CO2 (2×20 ml). The organic phases were combined and extracted with water (2×20 ml), 2.5% NaOH solution (2×30 ml) and water (2×20 ml). The organic phase was dried over Na2SO4 and evaporated. Yield was 12.0 g.

WORKUP

后处理

  1. stirringstirred for 5 minutes
  2. customThe phases were separated
  3. washthe aqueous phase was washed with CH2CO2 (2×20 ml)
  4. extractionextracted with water (2×20 ml), 2.5% NaOH solution (2×30 ml) and water (2×20 ml)
  5. dry with materialThe organic phase was dried over Na2SO4
  6. customevaporated