HRID1170068

反应详情

EQUATION

反应方程式

HRID 1170068 的结构方程式

PROCEDURE

实验过程

To a stirred solution of 1 M vinyl magnesium bromide in THF (9.1 L), 3-chloropropyl dimethylchlorosilane (1.5 Kg) was added over the period of 3 hr through an addition. The reaction mixture stirred further for 2 hr. Added D.M water (9.1 L) and separated the organic layer. The hazy aqueous layer was filtered through hyflo bed and extracted with dichloromethane (3.0 L). The dichloromethane extract was mixed with organic layer and evaporated to dryness to give yellow liquid which was distilled using a Vigreaux column to get pure colorless title product (0.986 Kg)

WORKUP

后处理

  1. customAdded D.M water (9.1 L) and separated the organic layer
  2. filtrationThe hazy aqueous layer was filtered through hyflo bed
  3. extractionextracted with dichloromethane (3.0 L)
  4. extractionThe dichloromethane extract
  5. additionwas mixed with organic layer
  6. customevaporated to dryness
  7. customto give yellow liquid which
  8. distillationwas distilled