反应详情

To a solution of 8-(1-ethyl-propyl)-3-(3-methoxy-thiophen-2-yl)-2,6-dimethyl-imidazo[1,2-b]pyridazine (0.78 g, 2.37 mmol) and CH2Cl2 (10 mL) is added NBS (0.44 g, 2.49 mmol). The solution is stirred for 1 hour, washed with water (3×10 mL), concentrated and purified by ISCO column chromatography (5%-15% EtOAc/hexane gradient) to furnish the title compound (0.87 g, 2.13 mmol, 90%). 1H NMR (CDCl3) δ 0.85 (t, J=7.5 Hz, 6H), 1.71-1.89 (m, 4H), 2.46 (s, 3H), 2.52 (s, 3H), 3.25-3.35 (m, 1H), 3.82 (s, 3H), 6.65 (s, 1H), 6.97 (s, 1H). LC/MS (m/z): calcd. for C18H22BrN3OS (M+H)+: 408.1; found: 408.3.

1. washwashed with water (3×10 mL)
2. concentrationconcentrated
3. custompurified by ISCO column chromatography (5%-15% EtOAc/hexane gradient)