反应详情

温度

0 °C

To a stirred slurry of 14.6 g. (0.11 mole) of aluminum chloride in 1,2-dichloroethane maintained at 0° C. were added 18.7 g. (0.11 mole) of 4-methoxybenzoyl chloride. The mixture was stirred at 0° C. for 10 minutes, and 21.0 g. (0.1 mole) of 3-phenylbenzothiophene in 1,2-dichloroethane were added. The mixture was stirred for two hours, the temperature being maintained at 0° C. The reaction mixture then was poured into a mixture of hydrochloric acid in ice. The resulting mixture was extracted with ether. The ether extract was washed with water, dilute aqueous sodium bicarbonate, and water. The ether layer was dried over magnesium sulfate, and the ether solvent was evaporated. The residue was dissolved in ethanol. The ethanol solution was filtered and maintained at 5° C. for three days. The resulting crystals were filtered and washed with ethanol and petroleum ether to obtain 23.7 g. (70 percent) of the title compound, m.p. 94°-95° C. The nmr spectrum was consistent with the structure of the title compound.

1. additionwere added 18.7 g
2. stirringThe mixture was stirred for two hours
3. temperaturethe temperature being maintained at 0° C
4. extractionThe resulting mixture was extracted with ether
5. extractionThe ether extract
6. washwas washed with water, dilute aqueous sodium bicarbonate, and water
7. dry with materialThe ether layer was dried over magnesium sulfate
8. customthe ether solvent was evaporated
9. dissolutionThe residue was dissolved in ethanol
10. filtrationThe ethanol solution was filtered
11. temperaturemaintained at 5° C. for three days
12. filtrationThe resulting crystals were filtered
13. washwashed with ethanol and petroleum ether
14. customto obtain 23.7 g