反应详情

温度

80 °C

A mixture of 2,5-difluorobenzonitrile (500 mg, 3.6 mmol), 1,2,4-triazole (273 mg, 3.9 mmol) and Cs2CO3 (1.27 g, 3.9 mmol) in DMF (10 mL) was heated at 80° C. for 2 days. The solvent was removed under reduced pressure. The residue was partitioned between H2O and EtOAc. The layers were separated and the aqueous layer extracted with EtOAc (×3). The combined organic extracts were washed with brine, dried over MgSO4, filtered and concentrated to give the title compound as an off white solid (596 mg) along with a minor bis-alkylated byproduct. 1H NMR (400 MHz, CDCl3): δ 8.71 (s, 1H), 8.19 (s, 1H), 7.75–7.98 (m, 1H), 7.48–7.57 (m, 2H).

1. customThe solvent was removed under reduced pressure
2. customThe residue was partitioned between H2O and EtOAc
3. customThe layers were separated
4. extractionthe aqueous layer extracted with EtOAc (×3)
5. washThe combined organic extracts were washed with brine
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated