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
Ferrocenoylvaleryl chloride (prepared as above and assumed to be 0.01 mole) was diluted with methylene chloride (10 mls.) and benzene (20 mls.) and the solution was cooled to 0°-5°. Aluminum chloride (2.6g; 0.02 mole) was then added with stirring over 30 minutes. After further stirring at room temperature for 2 hours, ice was added to the reaction mixture. The organic layer was then separated and washed successively with water, aqueous sodium bicarbonate solution, and water, before being dried over sodium sulphate. Evaporation under reduced pressure produced a brown oil from which chromatography on silica gel with toluene/ethyl acetate provided a pure sample of the required compound (0.32g; 9% yield) mp 135°-137°.
WORKUP
后处理
- temperaturethe solution was cooled to 0°-5°
- stirringAfter further stirring at room temperature for 2 hours
- additionice was added to the reaction mixture
- customThe organic layer was then separated
- washwashed successively with water, aqueous sodium bicarbonate solution, and water
- dry with materialbefore being dried over sodium sulphate
- customEvaporation under reduced pressure
- customproduced a brown oil from which chromatography on silica gel with toluene/ethyl acetate