HRID1637484

反应详情

EQUATION

反应方程式

HRID 1637484 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 4.40 g (110 mmol) of sodium hydroxide in 14 ml of water was added to a solution of 8.37 g (22.0 mmol) of diethyl 2-[1-(2,4-dimethoxyphenyl)hexyl]malonate (prepared as described in Preparation 2) in 50 ml of ethanol, and the resulting mixture was heated under reflux for 2.5 hours. At the end of this time, the reaction mixture was allowed to cool to room temperature, after which it was freed from ethanol by evaporation under reduced pressure. The resulting residue was acidified with concentrated hydrochloric acid and then extracted with ethyl acetate. The extract was washed with water and then with a saturated aqueous solution of sodium chloride, after which it was dried over anhydrous sodium sulfate. The solvent was removed by distillation under reduced pressure, to give 6.57 g of the title compound as a foam-like substance.

WORKUP

后处理

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 2.5 hours
  3. customafter which it was freed from ethanol by evaporation under reduced pressure
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with water
  6. dry with materialwith a saturated aqueous solution of sodium chloride, after which it was dried over anhydrous sodium sulfate
  7. customThe solvent was removed by distillation under reduced pressure