反应详情

A solution of 2-nitrobenzaldehyde (5.0 g, 33.1 mmol) and ammonium acetate (2.55 g, 33.1 mmol) in AcOH (20 mL) was treated dropwise at 20° C. with nitroethane (2.84 mL, 39.7 mmol). The resulting solution was heated under reflux for 2 h, then cooled and diluted with EtOAc. The organic layer was washed with saturated aqueous NaHCO3 solution and brine, then dried over Na2SO4. Filtration and removal of the volatiles gave a residue that was purified on silica gel (gradient elution, 0-40% EtOAc/hexanes) to give the title compound as an oil (2.3 g, 33%). LCMS (ES+) m/z 209 (M+H)+.

1. temperatureThe resulting solution was heated
2. temperatureunder reflux for 2 h
3. temperaturecooled
4. washThe organic layer was washed with saturated aqueous NaHCO3 solution and brine
5. dry with materialdried over Na2SO4
6. filtrationFiltration and removal of the volatiles
7. customgave a residue that
8. customwas purified on silica gel (gradient elution, 0-40% EtOAc/hexanes)