反应详情

温度

70 °C

53 Grams of 60% sodium hydride was gradually added to a solution prepared by dissolving 256.2 g of cyclohexyl 3,5-dimethyl-2-hydroxyphenyl ketone in 1 liter of dimethylformamide with stirring, generating heat at 70° C. After continuation of stirring for 30 minutes, the reaction mixture was cooled to room temperature and thereto was added dropwise 233 g of methyl iodide. The reaction mixture was further stirred at the same temperature for 2 hours and then added to 1 liter of ice water and stirred. The organic layer was extracted with 3 liters of ethyl acetate. The extract was washed with water and then with a saturated aqueous sodium chloride solution and then dried with anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 285.2 g of cyclohexyl 3,5-dimethyl-2-methoxyphenyl ketone.

1. customprepared
2. stirringAfter continuation of stirring for 30 minutes
3. temperaturethe reaction mixture was cooled to room temperature
4. stirringThe reaction mixture was further stirred at the same temperature for 2 hours
5. stirringstirred
6. extractionThe organic layer was extracted with 3 liters of ethyl acetate
7. washThe extract was washed with water
8. dry with materialwith a saturated aqueous sodium chloride solution and then dried with anhydrous magnesium sulfate
9. distillationThe solvent was distilled off under reduced pressure