HRID21420

反应详情

EQUATION

反应方程式

HRID 21420 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

tert-Butyldimethylsilylchloride (100 g, 0.66M) in dry dichloromethane (70 ml) was added, drop-wise, to a stirred mixture of distilled ethylene glycol (205.6 g, 3.31M), dry dichloromethane (200 ml), triethylamine (120 ml, 0.86M) and 4-dimethylaminopyridine (8 g, 0.066M) at 0° C. under a nitrogen atmosphere. After the addition the mixture was allowed to warm to ambient temperature and was stirred for a further 3 hours. The mixture was then filtered and the filtrate washed with dilute sodium bicarbonate solution, brine, dried over magnesium sulphate, filtered and then evaporated in vacuo to give a pale yellow oil.

WORKUP

后处理

  1. additionAfter the addition the mixture
  2. filtrationThe mixture was then filtered
  3. washthe filtrate washed with dilute sodium bicarbonate solution, brine
  4. dry with materialdried over magnesium sulphate
  5. filtrationfiltered
  6. customevaporated in vacuo
  7. customto give a pale yellow oil