反应详情

温度

23 °C

A heterogeneous mixture of (3-(4-(1H-pyrazol-1-yl)benzyl)-4-chloro-2-methoxyquinolin-6-yl)(1,2-dimethyl-1H-imidazol-5-yl)methanol (625 mg, 1.32 mmol, Intermediate 21: step a) and manganese dioxide (809 mg, 7.91 mmol) in dioxane (13 mL) was heated to 100° C. After 135 minutes, the flask was allowed to cool to 23° C. Dichloromethane (40 mL) was added and the mixture was filtered through Celite®, rinsing with dichloromethane. Silica gel (3 g) was added to the filtrate and the solvent was removed by rotary evaporation to afford a free-flowing powder. The powder was loaded onto a column of silica gel for purification. Elution with 30% ethyl acetate-hexanes initially, grading to 100% ethyl acetate provided the title compound as an off-white solid.

1. filtrationthe mixture was filtered through Celite®
2. washrinsing with dichloromethane
3. additionSilica gel (3 g) was added to the filtrate
4. customthe solvent was removed by rotary evaporation
5. customto afford a free-flowing powder
6. customThe powder was loaded onto a column of silica gel for purification
7. washElution with 30% ethyl acetate-hexanes initially