反应详情

温度

5 °C

To a suspension of 1,1-dimethylnitroethane (261.2 mg, 2.53 mmol) and zinc (247.0 mg, 3.78 mmol) in ethanol (3.0 ml) was added acetic acid (451.8 mg, 7.52 mmol) dropwise at 5° C. while stirring. The mixture was stirred at room temperature for 30 minutes. After cooling the mixture to 5° C. again, 4-(1-imidazolyl)benzaldehyde (216.5 mg, 1.26 mmol) was added dropwise to the mixture while stirring and stirred at room temperature overnight. Zinc acetate in the mixture was filtered off and the filtrate was concentrated and purified by silica gel chromatography (chloroform/methanol=10/1).

1. stirringThe mixture was stirred at room temperature for 30 minutes
2. stirringwhile stirring
3. stirringstirred at room temperature overnight
4. filtrationZinc acetate in the mixture was filtered off
5. concentrationthe filtrate was concentrated
6. custompurified by silica gel chromatography (chloroform/methanol=10/1)