反应详情

温度

90 °C

To a solution of 2,4-difluorobenzonitrile (10 g, 72 mmol), dissolved in THF (20 mL) and DMF (40 mL), was added 1,2,4-triazole sodium salt (6.3 g, 70 mmol) and the resulting mixture stirred at 90° C. for 3 h, after which it was filtered and concentrated. The remaining residue was adsorbed onto silica gel and purified by flash column chromatography eluting with 0%–30% ethyl acetate/hexanes to give the title compound as colorless needles (2.46 g, 18% yield). 1H NMR (500 MHz, CDCl3) δ ppm: 8.89 (1H, s), 8.19 (1H, s), 7.85 (1H, dd, J=8.7, 5.6 Hz), 7.60 (1H, dd, J=8.8, 2.4 Hz), 7.28–7.24 (1H, m). LCMS (M+H) calcd for C9H6N4F: 189.05; found: 189.13.

1. filtrationafter which it was filtered
2. concentrationconcentrated
3. custompurified by flash column chromatography
4. washeluting with 0%–30% ethyl acetate/hexanes