HRID1269947

反应详情

EQUATION

反应方程式

HRID 1269947 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Under a nitrogen atmosphere, ammonium chloride (4.17 g, 0.078 mol) and potassium cyanide (6.77 g, 0.104 mol) were added to a solution of 2-cyclohexen-1-one (5.0 g, 0.052 mol) in a 15%-aqueous N,N-dimethylformamide solution (60 ml) at room temperature, and the resulting mixture was heated to 100° C. After 3 hours, the reaction solution was poured into water and extracted with chloroform, and the organic layer was dried over anhydrous magnesium sulfate. The organic layer dried was concentrated under reduced pressure and the resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate) to obtain 1-cyanocyclohexan-3-one (345.4 mg, 5.4%).

WORKUP

后处理

  1. extractionextracted with chloroform
  2. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  3. customThe organic layer dried
  4. concentrationwas concentrated under reduced pressure
  5. customthe resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate)