HRID840994

反应详情

EQUATION

反应方程式

HRID 840994 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A mixture of 2-chlorobenzaldehyde (25.0 g, 178 mmol), acetone (40 ml) and water (20 ml) was cooled to 0° C., followed by adding dropwise thereto a 5% aqueous sodium hydroxide solution (7 ml), and the resulting mixture was stirred at room temperature for 4 hours. The reaction mixture was adjusted to pH 1 with 1N hydrochloric acid and extracted with ethyl acetate. The extract solution was washed with water and a saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure and the resulting residue was purified by a silica gel column chromatography to obtain 13.2 g of 1-(2-chlorophenyl)-1-buten-3-one.

WORKUP

后处理

  1. additionby adding dropwise
  2. extractionextracted with ethyl acetate
  3. washThe extract solution was washed with water
  4. dry with materiala saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate
  5. distillationThe solvent was distilled off under reduced pressure
  6. customthe resulting residue was purified by a silica gel column chromatography