反应详情

温度

80 °C

To a solution of sodium methoxide (23 g) in ethanol (150 mL) were added diethyl ethoxymethylene malonate (32.7 g) and isopropyl hydrazine (11.2 g) at room temperature. The mixture was stirred at 80° C. for 4 hours and stirred at 100° C. for another 2 hours. The reaction mixture was poured into 2 mol/L hydrochloric acid (300 mL). After the mixture was diluted with brine, the mixture was extracted with ethyl acetate. The organic layer was washed with brine and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure and the obtained residue was purified by column chromatography on silica gel (eluent: ethyl acetate/hexane=1/5) to give 10.5 g of the title compound.

1. stirringstirred at 100° C. for another 2 hours
2. extractionthe mixture was extracted with ethyl acetate
3. washThe organic layer was washed with brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customThe solvent was removed under reduced pressure
6. customthe obtained residue was purified by column chromatography on silica gel (eluent: ethyl acetate/hexane=1/5)