反应详情

A solution of ethyl α-(2-butenyl)-3-nitro-β-oxobenzenepropanoate (411 mg, 1.41 mmol) in 1,4-dioxane (12 mL) was stirred at 25° for 8.5 h under a hydrogen atmosphere (1 atm) in presence of Pd/BaSO4 (225 mg+150 mg added after 5.5 h). The suspension was filtered (50μ filter) and the filtrate was concentrated under reduced pressure. The residue was purified by flash chromatography (40-63μ silica gel, hexane:EtOAc, 3:1) to give ethyl 3-amino-α-butyl-β-oxobenzenepropionate (242 mg, 65% yield):

1. filtrationThe suspension was filtered
2. filtration(50μ filter)
3. concentrationthe filtrate was concentrated under reduced pressure
4. customThe residue was purified by flash chromatography (40-63μ silica gel, hexane:EtOAc, 3:1)