HRID2261877

反应详情

EQUATION

反应方程式

HRID 2261877 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
31 °C

PROCEDURE

实验过程

To a solution of silver nitrate (14.17 g, 0.0838 moles) dissolved in 200 ml water, 100 gm (0.419 moles) trans-4-(4-chlorophenyl)cyclohexane carboxylic acid and acetonitrile (500 ml) was added. The solution was heated to reflux followed by addition of 1,4-naphthoquinone (80 gm, 0.506 moles). A solution of ammonium persulfate (239 g; 1.048 moles) in water (600 ml) was added dropwise to the above solution and continued reflux for half an hour. The reaction mass was then cooled to 30-32° C. and extracted with methylene chloride. The organic layer was first washed with water, followed with 10% sodium carbonate aqueous solution, and further with water until neutral pH. The organic layer was concentrated to afford the compound of Formula II (2-[4-(4-chlorophenyl)cyclohexyl]-1,4-naphthoquinone, 149 gm).

WORKUP

后处理

  1. temperatureThe solution was heated
  2. temperatureto reflux
  3. temperaturecontinued reflux for half an hour
  4. extractionextracted with methylene chloride
  5. washThe organic layer was first washed with water
  6. concentrationThe organic layer was concentrated