反应详情

温度

65 °C

To a flask containing 3-(4-bromo-3-methyl-thiophen-2-yl)-8-(1-ethyl-propyl)-2,6-dimethyl-imidazo[1,2-b]pyridazine (0.25 g, 0.64 mmol) and PdCl2(dppf) (0.023 g, 0.032 mmol) is added a 0.5 M solution of 2-thiazolylzinc bromide (3.82 mL, 1.91 mmol). The solution is heated at 65° C. overnight, diluted with EtOAc (30 mL), washed with sat. NH4Cl (25 mL), dried over MgSO4, filtered and concentrated. The residue is purified by ISCO (15%-20% EtOAc gradient) furnish the title compound (0.19 g, 0.48 mmol, 76%). 1H NMR (CDCl3) δ 0.88 (t, J=7.5 Hz, 6H), 1.75-1.92 (m, 4H), 2.36 (s, 3H), 2.47 (s, 3H), 2.50 (, 3H), 3.29-3.39 (m, 1H), 6.69 (s, 1H), 7.33 (d, J=3.3 Hz, 1H), 7.89 (d, J=3.3 Hz, 1H), 7.99 (s, 1H). LC/MS (m/z): calcd. for C21H24N4S2 (M+H)+: 397.2; found: 397.3.

1. washwashed with sat. NH4Cl (25 mL)
2. dry with materialdried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated
5. customThe residue is purified by ISCO (15%-20% EtOAc gradient)