反应详情

A flask is charged with 5-(6-chloroimidazo[1,2-b]pyridazin-2-yl)-2-ethylaniline (4.00 g, 0.0146 mol), acetonitrile (120 mL) and pyridine (3.54 mL, 0.0438 mol). The mixture is stirred and trimethylacetyl chloride (1.98 mL, 0.0161 mol) is added and the mixture stirred for 16 hr at room temp. When the reaction is complete the mixture is diluted with water (500 mL) and stirred for 1 hour, and solid collected, washed with water (3×50 mL). Crude product is purified by silica gel chromatography (0-50% EtOAc in CH2Cl2) to give the title compound (4.8 g, 92%). LCMS m/z=357.5, 359.4 [M+H]+, tR=2.57 min.

1. stirringthe mixture stirred for 16 hr at room temp
2. stirringstirred for 1 hour
3. customsolid collected
4. washwashed with water (3×50 mL)
5. customCrude product is purified by silica gel chromatography (0-50% EtOAc in CH2Cl2)