反应详情

A mixture of 2,3-dichloro-1,4-naphthoquinone (57.0 gm), 4-(4-chlorophenyl)-cyclohexane-1-carboxylic acid (60.0 gm) and silver nitrate (42.7 gm) is taken in acetonitrile (600 ml) and then a solution of ammonium persulphate (180.12 gm) in water (780 ml) is added. The mixture is heated to reflux, maintaining good stirring. The mixture was refluxed for 4 hrs. Then cooled in ice for about 1 hr after which it is filtered. The filtrate is kept aside for acetonitrile recovery. The solid is extracted with hot methylene chloride (100 ml×3). The inorganic salt is collected separately for recovery of silver. The organic layer is dried over anhydrous sodium sulphate and concentrated to get light brownish yellow solid (38.5 gm).

1. temperatureThe mixture is heated
2. temperatureto reflux
3. temperaturemaintaining good stirring
4. temperatureThe mixture was refluxed for 4 hrs
5. temperatureThen 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. customThe inorganic salt is collected separately for recovery of silver
9. dry with materialThe organic layer is dried over anhydrous sodium sulphate
10. concentrationconcentrated