反应详情

温度

130 °C

Methyl 5-bromo-4-fluoro-2-methoxy-3-nitrobenzoate (I-229) (1.0 g, 3.25 mmol) was dissolved in acetic acid (10 ml), and at room temperature, iron powder (544 mg, 9.74 mmol) was added, followed by stirring at 130° C. for 4 hours. After cooling to room temperature, the insoluble matter was separated by filtration with washing with ethyl acetate. The organic layer of the filtrate was evaporated under reduced pressure, and the resulting residue was fractionated with ethyl acetate and aqueous 1 M sodium hydroxide solution. The organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated away, and the resulting residue was purified by middle-pressure liquid chromatography (eluent, hexane:ethyl acetate=4:1) to obtain the entitled compound (798 mg, 88%) as a colorless gel substance.

1. temperatureAfter cooling to room temperature
2. customthe insoluble matter was separated by filtration
3. washwith washing with ethyl acetate
4. customThe organic layer of the filtrate was evaporated under reduced pressure
5. washThe organic layer was washed with saturated brine
6. dry with materialdried over anhydrous sodium sulfate
7. customThe solvent was evaporated away
8. customthe resulting residue was purified by middle-pressure liquid chromatography (eluent, hexane:ethyl acetate=4:1)