反应详情

To a mixed solution comprising 500 ml of acetic acid, 50 ml of carbon tetrachloride, 50 ml of concentrated sulfuric acid, and 100 ml of water were added 58.5 g of the (trans-4-(2-(trans-4-n-propylcyclohexyl)ethyl)cyclohexyl)benzene mentioned above, 22.1 g of iodine, and 18.4 g of iodic acid, and the mixture was stirred under a reflux for 2 hours. After cooled, the mixture was washed with a saturated aqueous solution of sodium thiosulfate. Organic layer was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under a reduced pressure to obtain a yellow-brown oily product. This product was purified by a column chromatography over an alumina by using heptane as an eluent. Further, it was recrystallized from heptane to obtain 9.7 g of 4-(trans-4-(2-(trans-4-n-propylcyclohexyl)ethyl)cyclohexyl)iodobenzene.

1. temperaturea reflux for 2 hours
2. temperatureAfter cooled
3. washthe mixture was washed with a saturated aqueous solution of sodium thiosulfate
4. washOrganic layer was washed with water
5. dry with materialdried over anhydrous magnesium sulfate
6. distillationthe solvent was distilled off under a reduced pressure
7. customto obtain a yellow-brown oily product
8. customThis product was purified by a column chromatography over an alumina
9. customFurther, it was recrystallized from heptane