HRID233335

反应详情

EQUATION

反应方程式

HRID 233335 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of freshly prepared 2-chloro-2-oxo-1,3,2-dioxaphospholane (14.2 g, 0.1M) in dry dichloromethane (30 ml) was added, drop-wise, to a stirred mixture of 2-(tert-butyldimethylsilyloxy)ethanol (17.6 g, 0.1M), triethylamine (18.1 ml), 0.13M) in dry dichloromethane (30 ml) at 0° C. under a nitrogen atmosphere. The mixture was allowed to warm to ambient temperature and was stirred for a further 2 hours. The mixture was filtered and the filtrand washed with n-hexane. The filtrate was evaporated in vacuo, diluted with n-hexane (30 ml) filtered and the filtrate evaporated in vacuo to give a brown oil.

WORKUP

后处理

  1. filtrationThe mixture was filtered
  2. washthe filtrand washed with n-hexane
  3. customThe filtrate was evaporated in vacuo
  4. additiondiluted with n-hexane (30 ml)
  5. filtrationfiltered
  6. customthe filtrate evaporated in vacuo
  7. customto give a brown oil