反应详情

5-Amino-6-fluoro-4-methoxybiphenyl-3-carbonitrile (I-234) (500 mg, 2.06 mmol) was dissolved in acetic acid (9.5 ml), and at room temperature, N-bromosuccinimide (441 mg, 2.48 mmol) was gradually added. After stirring under nitrogen atmosphere at room temperature for 1 hour, the solvent was evaporated away under reduced pressure. The residue was fractionated with ethyl acetate and aqueous 1M sodium hydroxide solution. The organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate. After filtration, the solvent was evaporated away, and the resulting residue was purified by middle-pressure liquid chromatography (eluent, hexane:ethyl acetate=3:1) to obtain the entitled compound (592 mg, 89%) as a pale brown solid.

1. customthe solvent was evaporated away under reduced pressure
2. washThe organic layer was washed with saturated brine
3. dry with materialdried over anhydrous sodium sulfate
4. filtrationAfter filtration
5. customthe solvent was evaporated away
6. customthe resulting residue was purified by middle-pressure liquid chromatography (eluent, hexane:ethyl acetate=3:1)