反应详情

To a liquid mixture comprising 50 ml of acetic acid, 5 ml of carbon tetrachloride, 5 ml of concentrated sulfuric acid, and 10 ml of water, were added 5.8 g of the (2-(trans-4-(4-n-propylphenyl)cyclohexyl)ethyl)benzene mentioned above, 2.4 g of iodine, and 2 g of iodic acid, and they were 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, and further recrystallized from heptane to obtain 5.8 g of 4-(2-(trans-4-(4-n-propylphenyl)cyclohexyl)ethyl)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 recrystallized from heptane