反应详情

温度

120 °C

To a solution of 5-(4-chloro-thiophen-2-yl)-1-(2,2,2-trifluoro-ethyl)-1H-[1,2,4]triazole (1.13 g, 4.22 mmol) and AcOH (10 mL) in a sealed tube, is added Br2 (0.23 mL, 4.43 mmol). The solution is heated at 120° C. for 2 hours, and 140° C. for 5 hours. The solution is concentrated, diluted with Et2O (150 mL), washed with sat NaHCO3 (75 mL), sat. Na2S2O3 (75 mL), brine (75 mL) dried over MgSO4, filtered and concentrated. The residue is purified by ISCO flash chromatography (5%-15% EtOAc gradient) furnish the title compound (1.04 g, 3.00 mmol, 71%). 1H NMR (CDCl3) δ 4.88 (q, J=16.0, 7.9 Hz, 2H), 7.22 (s, 1H), 7.99 (s, 1H). LC/MS (m/z): calcd. for C8H4BrClF3N3S (M+H)+: 345.9; found: 346.0.

1. concentrationThe solution is concentrated
2. additiondiluted with Et2O (150 mL)
3. washwashed with sat NaHCO3 (75 mL), sat. Na2S2O3 (75 mL), brine (75 mL)
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue is purified by ISCO flash chromatography (5%-15% EtOAc gradient)