HRID1087756

反应详情

EQUATION

反应方程式

HRID 1087756 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A 125 ml round bottom flask equipped with a Dean-Stark trap was charged with 10 g of 1,2-dodecanediol, 7.1 g of diethyl carbonate and 50 ml of benzene. The solution was stirred until homogeneous and then 50 mg of 60% NaH was added. The reaction mixture was refluxed for 6 hours and then concentrated to afford 12.2 g of oil. This was taken up in 100 ml of pet. ether and allowed to crystallize in freezer whereupon 1.1 g of starting diol was recovered. Concentration of the filtrate gave 9.53 g (89.66%) of a colorless oil.

WORKUP

后处理

  1. customA 125 ml round bottom flask equipped with a Dean-Stark trap
  2. additionwas added
  3. temperatureThe reaction mixture was refluxed for 6 hours
  4. concentrationconcentrated