反应详情

A solution of 2-cyano-5-methylthiophene (compound 3-2, 3.0 g, 24 mmol), N-bromosuccinimide (Aldrich, 4.8 g, 27 mmol), and 2,2′-azobisisobutyronitrile (Aldrich, 0.4 g, 2.4 mmol) in CCl4 (Aldrich, 60 ml) was heated at reflux for 5 hours. After cooling to ambient temperature, the solvent was removed under vacuum to give a yellow oil. The oil was purified by a flash column chromatography (1:1 hexane/ethyl acetate) to give the title compound (4.5 g, 91%). TLC: Rf 0.91 (1:1 of hexane/ethyl acetate); 1H NMR (CDCl3): δ 4.66 (s, 2H), 7.10 (d, 1H, J=3.8 Hz), 7.48 (d, 1H, J=3.8 Hz).

1. temperatureat reflux for 5 hours
2. customthe solvent was removed under vacuum
3. customto give a yellow oil
4. customThe oil was purified by a flash column chromatography (1:1 hexane/ethyl acetate)