反应详情

温度

60 °C

To a suspension of diphosphorus pentoxide (70.0 g, 433 mmol) in acetonitrile (200 mL) was added a solution of methyl 4-[(2-ethoxy-2-oxoethyl)amino]-4-oxobutanoate (20.0 g, 92.1 mmol) in acetonitrile (50 mL) at room temperature under an argon gas atmosphere. The mixture was stirred at 60° C. for 1 hr and poured into saturated brine (1.5 L), and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (ethyl acetate/hexane=0/100→30/70) to give the title compound (7.06 g, yield 38%).

1. extractionthe mixture was extracted with ethyl acetate
2. dry with materialThe extract was dried over anhydrous sodium sulfate
3. customThe solvent was evaporated under reduced pressure
4. customthe residue was purified by silica gel column chromatography (ethyl acetate/hexane=0/100→30/70)