HRID905143

反应详情

EQUATION

反应方程式

HRID 905143 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A suspension of 1.50 g (6.14 mmol) of 2-(2',5'-dimethylphenyl)-5,5-dimethyl-1,3-cyclohexanedione in 15 ml of dry benzene was prepared and 0.49 g (7.37 mmol) of 85% powdered potassium hydroxide was added, followed by 1 drop of dicyclohexyl-18-crown-6-ether. After stirring for 30 minutes, 1.20 g (7.37 mmol) of 2-ethylhexanoyl chloride was added, and the reaction mixture refluxed for 12 hrs. The reaction mixture was cooled to room temperature, taken up in 150 ml ether and 50 ml of water, washed three times with 0.25 N, NaOH, two times with water, two times with 6 N HCl, and once more with water. The ether solution was dried and stripped to leave 2.10 g (92% yield) of 3-(2-ethylhexanoyloxy)-5,5-dimethyl-2-(2',5'-dimethylphenyl)-2-cyclohexenone as a clear, colorless oil.

WORKUP

后处理

  1. customwas prepared
  2. additionwas added
  3. temperaturethe reaction mixture refluxed for 12 hrs
  4. wash50 ml of water, washed three times with 0.25 N, NaOH, two times with water, two times with 6 N HCl
  5. dry with materialThe ether solution was dried