HRID536542
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
An amount of 160 mg (0.72 mmol) of the compound from Example 22A was heated under reflux with 129 mg (0.72 mmol) of N-bromosuccinimide and also 12 mg (0.07 mmol) of 2,2′-azobis-2-methylpropanenitrile in 5 ml of carbon tetrachloride for 16 h. After cooling to RT, the mixture was diluted with 10 ml of dichloromethane and washed with 10 ml of water. It was dried over sodium sulphate, filtered and concentrated under reduced pressure. The crude product was subsequently purified by chromatography [Method 8]. This gave 103 mg (47% of theory) of the target compound.
WORKUP
后处理
- washwashed with 10 ml of water
- dry with materialIt was dried over sodium sulphate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe crude product was subsequently purified by chromatography [Method 8]