HRID1461131

反应详情

EQUATION

反应方程式

HRID 1461131 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

A tetrahydrofuran solution of 3,7-dimethyloctylmagnesium bromide was prepared from 6.64 g (0.03 mol) of 3,7-dimethyloctyl bromide, 0.73 g of metallic magnesium, 50 ml of tetrahydrofuran and 3 droplets of ethylene dibromide in a similar manner to that described in Example 1 and cooled to 5° C., followed by the addition of 0.6 g (0.003 mol) of CuBr·(CH3)2S. The obtained mixture was stirred at that temperature for 30 minutes. 50 ml of a solution of 3.4 g (0.02 mol) of 3-chloro-6-methylene-2-methyloctadiene-1,7 having a purity of 70% in tetrahydrofuran was dropped into the resulting mixture over a period of 30 minutes. After the completion of the dropping, the obtained mixture was stirred at that temperature for one hour and subjected to TLC and HPLC to confirm the disappearance of the chlorine-containing raw material.

WORKUP

后处理

  1. stirringAfter the completion of the dropping, the obtained mixture was stirred at that temperature for one hour
  2. additioncontaining raw material