反应详情

温度

70 °C

Under a nitrogen atmosphere, an aqueous solution (10 ml) of ammonium chloride (2.37 g, 0.0443 mol) and an aqueous solution (20 ml) of potassium cyanide (3.15 g, 0.0483 mol) were added dropwise to a solution of 4,4-dimethyl-2-cyclohexen-1-one (5.0 g, 0.0403 mol) in N,N-dimethylformamide (30 ml) at room temperature, and the resulting mixture was heated to 70° C. After 2 hours, the reaction solution was poured into water and extracted with diethyl ether and then dichloromethane. The organic layer was dried over anhydrous magnesium sulfate. The organic layer dried was concentrated under reduced pressure and the resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate) to obtain 2,2-dimethyl-5-oxocyclohexanecarbonitrile (4.033 g, 66%).

1. extractionextracted with diethyl ether
2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
3. customThe organic layer dried
4. concentrationwas concentrated under reduced pressure
5. customthe resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate)