反应详情

温度

110 °C

A heterogeneous mixture containing 4-(3-(4-(1H-1,2,4-triazol-1-yl)benzyl)-2,4-dichloroquinoline-6-carbonyl)benzonitrile (583 mg, 1.20 mmol, Intermediate 16: step d), sodium methoxide (780 mg, 14.4 mmol), and toluene (17 mL) was heated to 110° C. After 45 minutes, the flask was allowed to cool to 23° C. Dichloromethane (100 mL) was added to the flask and then the mixture was filtered through Celite®, rinsing with dichloromethane. Silica gel (5 g) was added to the filtrate and the solvent was removed by rotary evaporation to provide a free-flowing powder. The powder was loaded onto a column of silica gel for flash chromatography purification. Elution with hexanes initially, grading to 80% ethyl acetate-hexanes afforded the title compound as a white solid.

1. temperatureto cool to 23° C
2. filtrationthe mixture was filtered through Celite®
3. washrinsing with dichloromethane
4. additionSilica gel (5 g) was added to the filtrate
5. customthe solvent was removed by rotary evaporation
6. customto provide a free-flowing powder
7. customThe powder was loaded onto a column of silica gel for flash chromatography purification
8. washElution with hexanes initially