反应详情

温度

110 °C

A heterogeneous mixture of 3-(4-(1H-pyrazol-1-yl)benzyl)-6-bromo-2,4-dichloroquinoline (13.0 g, 30.0 mmol, Intermediate 3: step c), sodium methoxide (9.73 g, 180 mmol), and toluene (120 mL) was heated at 110° C. After 5.5 hours, the mixture was cooled to room temperature then filtered through Celite® rinsing with dichloromethane. The filtrate was concentrated to provide a crude yellow solid. The crude solid was purified by flash column chromatography (silica gel, 50% dichloromethane-hexanes initially, grading to 100% dichloromethane) to provide the title compound as a white solid.

1. temperaturethe mixture was cooled to room temperature
2. filtrationthen filtered through Celite®
3. washrinsing with dichloromethane
4. concentrationThe filtrate was concentrated
5. customto provide a crude yellow solid
6. customThe crude solid was purified by flash column chromatography (silica gel, 50% dichloromethane-hexanes initially