反应详情

Crude 4-(2,3-difluoro-4-ethoxyphenyl)-cyclohexanone monoethylene acetal (50.3 mmol) obtained in Step 1 was dissolved in 200 ml of toluene, 87% formic acid (503 mmol) was added, and the solution was heated to reflux for 4 hours. The reaction solution was washed twice with 100 ml of a saturated aqueous solution of sodium hydrogen carbonate, then three times with 100 ml of water, and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, to form crude 4-(2,3-difluoro-4-ethoxyphenyl)-cyclohexanone (50.3 mmol).

1. temperaturethe solution was heated
2. temperatureto reflux for 4 hours
3. washThe reaction solution was washed twice with 100 ml of a saturated aqueous solution of sodium hydrogen carbonate
4. dry with materialthree times with 100 ml of water, and dried over anhydrous magnesium sulfate
5. distillationThe solvent was distilled off under reduced pressure