反应详情

温度

115 °C

A mixture of 3-(4-(1H-pyrazol-1-yl)benzyl)-6-bromo-2,4-dichloroquinoline (1.44 g, 3.33 mmol, Intermediate 3: step c) and diethylamine (6.91 mL, 66.5 mmol) in DMF (10 mL) in a sealed tube was heated in a 115° C. oil bath for 23 h. The mixture was diluted with EtOAc and extracted with water (5×, sat. aq. NaCl added as needed to achieve phase separation). The organic phase was dried (Na2SO4), filtered, and concentrated. The residue was purified by flash column chromatography (silica gel, dry loading, 2-10% EtOAc-heptanes first column, 0-4% EtOAc-heptanes second column) to afford the title compound as a white solid.

1. extractionextracted with water (5×, sat. aq. NaCl added as needed to achieve phase separation)
2. dry with materialThe organic phase was dried (Na2SO4)
3. filtrationfiltered
4. concentrationconcentrated
5. customThe residue was purified by flash column chromatography (silica gel, dry loading, 2-10% EtOAc-heptanes first column, 0-4% EtOAc-heptanes second column)