HRID329697

反应详情

EQUATION

反应方程式

HRID 329697 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The title compound was prepared using the method of Clark and Heathcock. J. Org. Chem., 1976, 41, 636. To a suspension of dimedone (15.0 g, 107 mmol) in chloroform (40 ml) was added slowly oxalyl chloride (27.2 g, 214 mmol). The addition was accompanied by vigorous evolution of gas. After stirring at room temperature for 10 minutes, the slurry was refluxed for 20 minutes to give a yellow solution which was evaporated and distilled to give 15.7 g (92%) of chloroenone as a colorless liquid, bp 72° (5 mm). ##STR5##

WORKUP

后处理

  1. additionThe addition
  2. temperaturethe slurry was refluxed for 20 minutes
  3. customto give a yellow solution which
  4. customwas evaporated
  5. distillationdistilled
  6. customto give 15.7 g (92%) of chloroenone as a colorless liquid, bp 72° (5 mm)