反应详情

温度

70 °C

To a solution of methyl 2-fluoro-3-nitrobenzoate (78 g) in THF (400 ml) and methanol (100 ml) was added Raney Ni (40 g), the mixture was heated to 70° C., and then 25 ml of hydrazine hydrate (N2H4H2O, 85%) was added dropwise. The reaction was monitored by TLC, when the starting material was totally consumed the addition of hydrazine was stop. The mixture was cooled to rt and filtered, the filtrate was concentrated under vacuum to leave a brown oil, which was purified by chromatography (SiO2, 300-400 mesh, PE:EtOAc=11:2) to afford the title compound was obtained as a yellow oil (45 g, 68%). 1H NMR (300 MHz, DMSO) δ ppm 6.96 (m, 3H), 5.36 (s, 2H), 3.81 (s, 3H).

1. customwas totally consumed
2. additionthe addition of hydrazine
3. temperatureThe mixture was cooled to rt
4. filtrationfiltered
5. concentrationthe filtrate was concentrated under vacuum
6. customto leave a brown oil, which
7. customwas purified by chromatography (SiO2, 300-400 mesh, PE:EtOAc=11:2)