反应详情

温度

125 °C

To a vial flushed with argon was added 4-bromo-2-hydrazinylpyridine (1.88 g, 10 mmol) and acetic acid (2.5 mL). The mixture was refluxed at 125° C. under argon for 16 hours. After cooling to room temperature, acetic acid was distilled off, and to the residue was added saturated NaHCO3 (150 mL) and DCM (150 mL). The aqueous layer was extracted with DCM, the organic extracts were combined, dried over MgSO4, and concentrated to give the product. 1H NMR (400 MHz, CDCl3) δ 7.95-7.90 (m, 1H), 7.73 (d, J=7.3 Hz, 1H), 6.94 (dd, J=7.3, 1.7 Hz, 1H), 2.74 (s, 3H).

1. customTo a vial flushed with argon
2. temperatureAfter cooling to room temperature
3. distillationacetic acid was distilled off
4. additionto the residue was added saturated NaHCO3 (150 mL) and DCM (150 mL)
5. extractionThe aqueous layer was extracted with DCM
6. dry with materialdried over MgSO4
7. concentrationconcentrated
8. customto give the product