反应详情

温度

120 °C

To a solution of 4-chloro-3-fluorobenzaldehyde (10 g, 63.07 mmol) and ammonium acetate (4.861 g, 63.07 mmol) in HOAc (50 mL) was added nitromethane (14.12 mL, 252.3 mmol) and the reaction mixture was heated to reflux (120° C. oil bath) for 18 h. The reaction was cooled and diluted with water. The reaction mixture was filtered and solids were purified by SiO2 chromatography eluting with a EtOAc/hexane gradient (0 to 5% EtOAc) to afford 1.736 g (13.65%) of (E)-1-chloro-2-fluoro-4-(2-nitrovinyl)benzene (86).

1. temperaturethe reaction mixture was heated
2. temperatureThe reaction was cooled
3. filtrationThe reaction mixture was filtered
4. customsolids were purified by SiO2 chromatography
5. washeluting with a EtOAc/hexane gradient (0 to 5% EtOAc)