تفاعل #45802

معادلة التفاعل

5-Amino-6-fluoro-4-methoxybiphenyl-3-carbonitrile

N-bromosuccinimide

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compound

المردود 89.5%

5-Amino-2-bromo-6-fluoro-4-methoxybiphenyl-3-carbonitrile

المردود 89.5%

المذيبات

acetic acid

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر