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
CONDITIONS
反应条件
- 温度
- 60 °C
PROCEDURE
实验过程
A mixture of 8-(2,6-dichlorobenzoylamino)-3-methylquinoline (104 mg), N-bromosuccinimide (67.1 mg) and 2,2'-azobis(2,4-dimethyl-4-methoxyvaleronitrile) (20.1 mg) in carbon tetrachloride (3 ml) was refluxed for 2 hours. After cooling, the mixture was washed with water, saturated sodium bicarbonate solution and brine, dried over magnesium sulfate and evaporated in vacuo to give a residue containing 3-bromomethyl-8-(2,6-dichlorobenzoylamino)quinoline. The residue was dissolved in ethylene chloride, and imidazole (64.1 mg) was added thereto. After stirring for 2.5 hours at 60° C., the mixture was washed with water and brine, dried over magnesium sulfate and evaporated in vacuo. The residue was purified by column chromatography on silica gel (ethyl acetate-dichloromethane) to give 8-(2,6-dichlorobenzoylamino)-3-(imidazol-1-ylmethyl)quinoline (36.2 mg).
WORKUP
后处理
- temperaturewas refluxed for 2 hours
- temperatureAfter cooling
- washthe mixture was washed with water, saturated sodium bicarbonate solution and brine
- dry with materialdried over magnesium sulfate
- customevaporated in vacuo
- customto give a residue
- washthe mixture was washed with water and brine
- dry with materialdried over magnesium sulfate
- customevaporated in vacuo
- customThe residue was purified by column chromatography on silica gel (ethyl acetate-dichloromethane)