反应详情

温度

100 °C

3.1 g of cis-2,6-dimethylcyclohexanoneoxime and 12 g of poly phosphoric acid were added to 40 ml of xylene and stirred at 100° C. for 10 hours. Then the reaction mixture which was cooled to about room temperature was added to ice-water. Potassium carbonate was added to it, and extracted with ethyl acetate three times. The organic layers were joined, washed with saturated aqueous solution of sodium chloride, dried with anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 2.5 g of hexahydro-cis-3,7-dimethylazepin-2-one.

1. temperatureThen the reaction mixture which was cooled to about room temperature
2. extractionextracted with ethyl acetate three times
3. washwashed with saturated aqueous solution of sodium chloride
4. dry with materialdried with anhydrous magnesium sulfate
5. concentrationconcentrated