反应详情

温度

90 °C

Methyl 5-chloro-2-(3-fluorophenyl)nicotinate 1-oxide (3.0 g, 11 mmol) was stirred in phosphoryl chloride (30 mL) and heated at 90° C. for 1 hour. Evaporation and purification by flash column chromatography using ethyl acetate in hexanes (0-20%) gave the desired compound (2.4 g, 75%). LCMS calculated for C13H9Cl2FNO2 (M+H)+: m/z=300.0, 302.0. found: 299.8, 301.8. 1H NMR (300 MHz, CDCl3): δ 8.23 (s, 1H), 7.40 (m, 2H), 7.22 (m, 1H), 7.17 (m, 1H), 3.73 (s, 3H).

1. customEvaporation and purification by flash column chromatography