HRID1416533

反应详情

EQUATION

反应方程式

HRID 1416533 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

5,8-Dimethyl-1,4-benzodioxane. To a stirred solution of 3 g of 3,6-dimethylcatechol and 6.15 g of potassium carbonate in 35 mL of ethylene glycol is added 3.74 mL of dibromoethane. A reflux condenser is attached and the mixture heated in an oil bath to 120° C. for 4 hours. The mixture is allowed to cool to room temperature and then is distributed between 100 mL of saturated potassium carbonate solution and 200 mL of ether. The ether layer is dried over magnesium sulfate and concentrated under reduced pressure to yield a red liquid, which is purified by chromatography on silica gel to afford 2.90 g of 5,8-dimethyl-1,3-benzodioxane as a light yellow liquid.

WORKUP

后处理

  1. customA reflux condenser is attached
  2. temperatureto cool to room temperature
  3. dry with materialThe ether layer is dried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto yield a red liquid, which
  6. customis purified by chromatography on silica gel