反应详情

15 g of 1-(4-Fluoro-phenyl)-4-oxo-cyclohexanecarbonitrile (12) were dissolved in 500 mL of toluene, then 900 mg of p-toluene sulfonic acid were added and the reaction mixture was heated in a Dean-Stark apparatus for 6 h. The mixture was allowed to cool to room temperature and washed twice with saturated aqueous sodium bicarbonate solution and brine, dried over magnesium sulphate and evaporated to dryness to yield 17.9 g of the desired product. Rt=1.47 min (Method 5). Detected mass: 262.2 (M+H+).

1. temperaturethe reaction mixture was heated in a Dean-Stark apparatus for 6 h
2. washwashed twice with saturated aqueous sodium bicarbonate solution and brine
3. dry with materialdried over magnesium sulphate
4. customevaporated to dryness