HRID1194299

反应详情

EQUATION

反应方程式

HRID 1194299 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

198 g (6.6 mol) of sodium hydride (80% strength) and 500 g of toluene are introduced into a flask, and the mixture is heated to the reflux temperature. 432 g (3 mol) of 7-octene-1,2-diol, dissolved in 1,500 g of toluene, are then added over 3 hours, and the mixture is stirred at the reflux temperature until hydrogen evolution is complete. 830 g (6.6 mol) of dimethyl sulphate are added over 4 hours, and the mixture is stirred for a further 2 hours. After addition of 50 ml of methanol, 1,500 g of water are added in order to dissolve the precipitate. The phases are separated and the organic phase is distilled. 420 g of 1,2-dimethoxyoct-7-ene having a boiling point of 80° C./10 mbar, corresponding to a yield of 81% of theory) are obtained.

WORKUP

后处理

  1. temperaturethe mixture is heated to the reflux temperature
  2. additionare then added over 3 hours
  3. additionare added in order
  4. dissolutionto dissolve the precipitate
  5. customThe phases are separated
  6. distillationthe organic phase is distilled