反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture is heated to the reflux temperature
- additionare then added over 3 hours
- additionare added in order
- dissolutionto dissolve the precipitate
- customThe phases are separated
- distillationthe organic phase is distilled