反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture is heated
- temperatureto reflux
- temperaturemaintaining good stirring
- temperatureThe mixture refluxed for 4 hrs
- temperatureThen it is cooled in ice for about 1 hr after which it
- filtrationis filtered
- extractionThe solid is extracted with hot methylene chloride (100 ml×3)
- dry with materialThe organic layer is dried over anhydrous sodium sulphate
- concentrationconcentrated
- customto get light brownish yellow solid
- customThis on crystallization from acetonitrile