反応 #45802

反応方程式

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

N-bromosuccinimide

→

compound

収率 89.5%

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

収率 89.5%

溶媒

acetic acid

反応条件

後処理

1. 1
   その他the solvent was evaporated away under reduced pressure
2. 2
   洗浄The organic layer was washed with saturated brine
3. 3
   乾燥dried over anhydrous sodium sulfate
4. 4
   ろ過After filtration
5. 5
   その他the solvent was evaporated away
6. 6
   その他the resulting residue was purified by middle-pressure liquid chromatography (eluent, hexane:ethyl acetate=3:1)

実験手順

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.

出典