反应详情

A mixture of 2-fluoro-4′-methylbiphenyl (8.70 g), N-bromosuccinimide (8.32 g), 2,2′-azobisisobutyronitrile (0.10 g) and carbon tetrachloride (150 ml) is refluxed by heating for five hours. The reaction solution is washed with water. The residue, which is obtained by concentrating the organic layer, is purified using silica gel column chromatography (eluate: hexane/ethyl acetate=9/1) and thus, preliminarily purified 2-fluoro-4′-bromomethylbiphenyl is obtained. Furthermore, crystallization using hexane produced 2-fluoro-4′-bromomethylbiphenyl (4.93 g). 1H-NMR (CDCl3, δ): 4.55 (2H, s), 7.13-7.23 (2H, m), 7.33 (1H, m), 7.43 (1H, m), 7.47 (2H, d, J=8.1 Hz), 7.54 (2H, d, J=8.1 Hz).

1. temperatureis refluxed
2. temperatureby heating for five hours
3. washThe reaction solution is washed with water
4. customThe residue, which is obtained
5. concentrationby concentrating the organic layer
6. customis purified