反应详情

A mixture of 3-bromo-1-(4-nitrophenyl)-1H-1,2,4-triazole (0.51 g, 1.9 mmol), SnCl2-2H2O (2.14 g, 9.5 mmol) and EtOH (4 mL) was heated at reflux for 4 h. The reaction mixture was cooled to room temperature and basified with NaOH (2M aq.) until pH 7˜9. The resulting precipitate was filtered through Celite and washed with EtOH. The EtOH filtrate was concentrated in vacuo and the crude residue was dissolved in water and extracted with EtOAc (3×). The combined organics were dried (MgSO4) and concentrated in vacuo to provide the desired product as a white solid. 1H NMR (CDCl3, 400 MHz) δ 8.28 (s, 1H), 7.40 (d, 2H), 6.79 (d, 2H), 3.90 (br s, 2H).

1. temperaturewas heated
2. temperatureat reflux for 4 h
3. filtrationThe resulting precipitate was filtered through Celite
4. washwashed with EtOH
5. concentrationThe EtOH filtrate was concentrated in vacuo
6. dissolutionthe crude residue was dissolved in water
7. extractionextracted with EtOAc (3×)
8. dry with materialThe combined organics were dried (MgSO4)
9. concentrationconcentrated in vacuo