HRID2061943

反应详情

EQUATION

反应方程式

HRID 2061943 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 2,3-dichloro-1,4-naphthoquinone (5 gm), trans 4-(4-chlorophenyl)-cyclohexane-1-carboxylic acid (6.06 gm) and silver nitrate (2.47 gm) is taken in acetonitrile (60 ml) and the mixture is heated to reflux, maintaining good stirring. Then a solution of ammonium persulphate (14.23 gm) in water (77 ml) is added through a dropping funnel over a period of 1-2 hrs. The mixture refluxed for 4 hrs. Then it is cooled in ice for about 1 hr after which it is filtered. The solid is extracted with hot methylene chloride (100 ml×3). The organic layer is dried over anhydrous sodium sulphate and concentrated to get light brownish yellow solid. This on crystallization from acetonitrile afforded the trans compound as yellow crystals (1.5 gm).

WORKUP

后处理

  1. temperaturethe mixture is heated
  2. temperatureto reflux
  3. temperaturemaintaining good stirring
  4. temperatureThe mixture refluxed for 4 hrs
  5. temperatureThen it is cooled in ice for about 1 hr after which it
  6. filtrationis filtered
  7. extractionThe solid is extracted with hot methylene chloride (100 ml×3)
  8. dry with materialThe organic layer is dried over anhydrous sodium sulphate
  9. concentrationconcentrated
  10. customto get light brownish yellow solid
  11. customThis on crystallization from acetonitrile