反应详情

温度

60 °C

To a solution of 2-(3-bromo-4-(trifluoromethyl)phenyl)-6-ethoxyimidazo[1,2-b]pyridazine (0.025 g, 0.0647 mmol) in THF (0.647 mL) containing pyridin-2-ylzinc(II) bromide (0.323 mmol) is added Pd(dppf)Cl2 (0.0194 mmol). The mixture is heated at 60° C. for 12 hours, then cooled, quenched with sat. aqueous NaHCO3 (1 mL) and extracted with CH2Cl2 (3×3 mL). Organic layer is collected and concentrated to dryness. The crude product is purified via preparative TLC using CH2Cl2:EtOAc:methanol (1:1:0.1) to afford 0.0022 g (9%) of the title compound as a white solid: Rf 0.35 (1:1 EtOAc:hexanes); LCMS (m/z)=385.4 [M+H]+, tR=2.69 min. (compound same as Example 218)

1. temperaturecooled
2. customquenched with sat. aqueous NaHCO3 (1 mL)
3. extractionextracted with CH2Cl2 (3×3 mL)
4. customOrganic layer is collected
5. concentrationconcentrated to dryness
6. customThe crude product is purified via preparative TLC