反应详情

温度

180 °C

Ethyl-5-bromo-4-[(1H-imidazol-2ylthio) methyl]-1-phenyl-1H-pyrazole-3-carboxylate (0.3 g, 0.74 mmol, 1 eq), Cul (14 mg, 0.074 mmol, 0.1 eq), N,N-dimethylglycine (15 mg, 0.147 mmol, 0.2 eq), K2CO3 (0.2 g, 1.47 mmol, 2 eq) are taken in DMSO (6 mL) heated at 180° C. for 0.5 h under microwave irradiation. The reaction mixture is diluted with DCM and filtered through a pad of celite. The filtrate is partitioned between DCM and water. The organic layer is washed with brine, dried over Na2SO4 and concentrated. The crude is purified by flash chromatography to afford the title compound. 1H NMR (DMSO-d6, 400 MHz): δ 7.67-7.59 (m, 5H), 6.93 (d, J=1.5 Hz, 1H), 6.48 (d, J=1.4 Hz, 1H), 4.40 (s, 2H), 4.34 (q, J=7.7 Hz, 2H), 1.31 (t, J=7.7 Hz, 3H). MS (ESI+): 313.2. HPLC (max plot) 97.73%; Rt 2.73 min.

1. filtrationfiltered through a pad of celite
2. customThe filtrate is partitioned between DCM and water
3. washThe organic layer is washed with brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. customThe crude is purified by flash chromatography