HRID1066550

反应详情

EQUATION

反应方程式

HRID 1066550 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of compound 39 (4.25 g, 0.022 mol), bromine (12.31 g, 0.077 mol) and chloroform (50 ml) was heated under reflux overnight. A further portion of bromine (12.31 g, 0.077 mol) was then added and heating continued for another 24 h. The resultant solution was washed with a saturated solution of sodium thiosulphate and finally with water. The dichloromethane solution was dried (MgSO4) and evaporated in vacuo and the crude oil was purified by column chromatography (10% petrol/dichloromethane) to yield a fawn oil.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux overnight
  3. temperatureheating
  4. washThe resultant solution was washed with a saturated solution of sodium thiosulphate and finally with water
  5. dry with materialThe dichloromethane solution was dried (MgSO4)
  6. customevaporated in vacuo
  7. customthe crude oil was purified by column chromatography (10% petrol/dichloromethane)
  8. customto yield a fawn oil