反应详情

A mixture of ethyl 2-(3,4-difluorophenyl)acetate (1.20 g, 5.99 mmol), N-bromosuccinimide (1.17 g, 6.59 mmol), and 2,2′-azobis(isobutyronitrile) (0.148 g, 0.899 mmol) in CCl4 (20 mL) was gradually heated to reflux and stirred at this temperature overnight. The solvent was removed in vacuum. The residue was purified by flash column chromatography (100% hexanes for 5 minutes, then 0 to 5% of EtOAc in hexanes over 23 minutes). The desired product was obtained as a colorless oil (1.14 g, 68%). 1H NMR (300 MHz, CDCl3) δ 1.31 (d, J=6.0 Hz, 3H), 4.17-4.35 (m, 2H), 5.27 (s, 1H), 7.11-7.20 (m, 1H), 7.24-7.30 (m, 1H), 7.42-7.52 (m, 1H).

1. temperaturewas gradually heated
2. temperatureto reflux
3. customThe solvent was removed in vacuum
4. customThe residue was purified by flash column chromatography (100% hexanes for 5 minutes
5. wait0 to 5% of EtOAc in hexanes over 23 minutes)