反应详情

温度

100 °C

Into 40 ml of xylene were added 3.1 g of cis-2,6-dimethylcyclohexanone oxime and 12 g of polyphosphoric acid, the mixture was stirred for 10 hours at 100° C. The reaction mixture was cooled to near room temperature, poured into ice-water. Sodium carbonate was added to the mixture, and the mixture was extracted with ethyl acetate three times. The organic layers was washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 2.5 g of cis-3,7-dimethylhexahydro-1H-azepine-2-one.

1. temperatureThe reaction mixture was cooled to near room temperature
2. extractionthe mixture was extracted with ethyl acetate three times
3. washThe organic layers was washed with a saturated sodium chloride aqueous solution
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated