反应详情

温度

100 °C

The starting material, 5-benzyloxy-2-fluoro-4-methylaniline, was obtained by adding iron powder (2.88 g, 51 mmol), in portions, to a solution of 5-benzyloxy-2-fluoro-4-methylnitrobenzene (4.8 g, 18 mmol) in acetic acid (33 ml) and water (5.7 ml), at ambient temperature. The mixture was heated and after stirring at 100° C. for 10 minutes, it was cooled and partitioned between ethyl acetate and water. The organic layer was washed with water, aqueous saturated sodium carbonate solution and then brine, dried (MgSO4) and the solvent evaporated. The residue was purified by flash chromatography using petroleum ether/ethyl acetate (8/2) as eluent to give 5-benzyloxy-2-fluoro-4-methylaniline (3.65 g, 87%).

1. customat ambient temperature
2. temperatureThe mixture was heated
3. temperatureit was cooled
4. custompartitioned between ethyl acetate and water
5. washThe organic layer was washed with water, aqueous saturated sodium carbonate solution
6. dry with materialbrine, dried (MgSO4)
7. customthe solvent evaporated
8. customThe residue was purified by flash chromatography