HRID1657510

反应详情

EQUATION

反应方程式

HRID 1657510 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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°. Aluminium 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 (0.32 g; 9% yield) mp 135°-7°.

WORKUP

后处理

  1. temperaturethe solution was cooled to 0°-5°
  2. stirringAfter further stirring at room temperature for 2 hours
  3. additionice was added to the reaction mixture
  4. customThe organic layer was then separated
  5. washwashed successively with water, aqueous sodium bicarbonate solution, and water
  6. dry with materialbefore being dried over sodium sulphate
  7. customEvaporation under reduced pressure
  8. customproduced a brown oil from which chromatography on silica gel with toluene/ethyl acetate