反应详情

25 g of 1-(4-Fluoro-phenyl)-4-oxo-cyclohexanecarbonitrile (73) were dissolved in 850 mL of toluene. 9 mL of ethylene glycol and 1.5 g of p-toluene sulfonic acid were added and the mixture was refluxed at a Dean-Stark apparatus for 6 h. The mixture was allowed to cool down to room temperature and extracted twice with saturated sodium bicarbonate solution and once with brine. The organic layer was dried over sodium sulfate and evaporated to dryness to give 30.15 g of crude product, that was sufficiently pure for further conversion. Rt=1.47 min (Method C). Detected mass: 262.2 (M+H+).

1. temperaturethe mixture was refluxed at a Dean-Stark apparatus for 6 h
2. extractionextracted twice with saturated sodium bicarbonate solution and once with brine
3. dry with materialThe organic layer was dried over sodium sulfate
4. customevaporated to dryness