HRID41667

反应详情

EQUATION

反应方程式

HRID 41667 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1-methyl-10-oxa-tricyclo[5.2.1.0*2,6*]decane-3,5-dione (3 g, 16.6 mmol) in chloroform (8 ml) is added PCl5 portionwise. The reaction mixture is stirred and heated at reflux for 5 hours. The reaction mixture is evaporated to dryness The crude product is purified by flash chromatography on silica gel to give 5-chloro-1-methyl-10-oxa-tricyclo[5.2.1.0*2,6*]dec-4-en-3-one (1.39 g).

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for 5 hours
  3. customThe reaction mixture is evaporated to dryness The crude product
  4. customis purified by flash chromatography on silica gel