反应详情

1-Ethyl-3-(3'-dimethylamino-propyl)carbodiimide (5.87 ml) was added to a mixture of 4-isopropylphenylhydrazine hydrochloride (5.0 g), acetic acid (1.84 ml), triethylamine (3.73 ml) and 1-hydroxybenzotriazole hydrate (40.4 mg) in dichloromethane (50 ml) under ice-cooling and then the mixture was stirred overnight at room temperature. After removal of solvent by evaporation, the resulting residue was partitioned between diluted hydrochloric acid and ethyl acetate. The organic layer was washed successively with aqueous sodium hydrogen carbonate solution, water, and brine, and was dried over magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to column chromatography on silica gel and eluted with a mixture of dichloromethane and methanol. The fractions containing the objective compound were combined and concentrated under reduced pressure to give 1-acetyl-2-(4-iso-propylphenyl)-hydrazine (3.00 g).

1. temperaturecooling
2. customAfter removal of solvent
3. customby evaporation
4. customthe resulting residue was partitioned between diluted hydrochloric acid and ethyl acetate
5. washThe organic layer was washed successively with aqueous sodium hydrogen carbonate solution, water, and brine
6. dry with materialwas dried over magnesium sulfate
7. concentrationconcentrated under reduced pressure
8. washeluted with a mixture of dichloromethane and methanol
9. additionThe fractions containing the objective compound
10. concentrationconcentrated under reduced pressure