HRID264552

反应详情

EQUATION

反应方程式

HRID 264552 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 23.9 g of 4-thiochromanone, 30 ml of 3-buten-2-ol and 240 mg of p-toluenesulfonic acid in 30 ml of 2,2-dimethoxy-propane and 240 ml of anhydrous toluene was boiled under reflux for 20 hours. The reaction mixture was subsequently concentrated in a vacuum and purified by column chromatography on silica gel (hexane/diethyl ether 5:1). 15.3 g (48%) of (RS)-2-(2-buten-1-yl)-4-thiochromanone were obtained as a yellow oil.

WORKUP

后处理

  1. temperatureunder reflux for 20 hours
  2. concentrationThe reaction mixture was subsequently concentrated in a vacuum
  3. custompurified by column chromatography on silica gel (hexane/diethyl ether 5:1)