HRID1250332
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
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
- temperaturewas heated
- temperatureunder reflux overnight
- temperatureheating
- washThe resultant solution was washed with a saturated solution of sodium thiosulphate and finally with water
- dry with materialThe dichloromethane solution was dried (MgSO4)
- customevaporated in vacuo
- customthe crude oil was purified by column chromatography (10% petrol/dichloromethane)
- customto yield a fawn oil