Aluminum → (4-Chloro-2-methoxy-3-(4-(trifluoromethyl)benzyl)quinolin-6-yl)(1,2-dimethyl-1H-imidazol-5-yl)methanone

温度

45 °C

To a 100 mL flask containing (4-chloro-2-methoxy-3-(4-(trifluoromethyl)benzyl)quinolin-6-yl)(1,2-dimethyl-1H-imidazol-5-yl)methanol (1.68 g, 3.53 mmol, Intermediate 49: step a) was added 1,4-dioxane (85 mL) to give a suspension at room temperature. Heating to approximately 45° C. formed a clear homogeneous solution. Then activated MnO2 (1.5 g, 17.2 mmol) was introduced and the mixture was heated to reflux in an aluminum heating mantle under an atmosphere of N2. After 70 minutes, the contents were cooled to 60° C. and then filtered through a Celite® pad and rinsed with THF. The resulting solution was concentrated and passed through a silica gel column (5% MeOH-DCM) to give the title compound as a white powder.

1. customto give a suspension at room temperature
2. customformed a clear homogeneous solution
3. temperaturethe mixture was heated
4. temperaturethe contents were cooled to 60° C.
5. filtrationfiltered through a Celite® pad
6. washrinsed with THF
7. concentrationThe resulting solution was concentrated

ORDレコード

ord-0cb78894e72843d28dd2470697242b43

出典データセット

uspto-grants-2016_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09290476B2