Dimethylformamide → Methyl 4-(5,5,5-trifluoro-2-(2-methyl-4-(5-(trifluoromethyl)pyridin-2-yl)phenyl)pentyl)benzoate

温度

80 °C

A reaction mixture of methyl 4-((4,4,4-trifluoro-1-(2-methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl)butyl)amino)benzoate (14.3 g) obtained in step F, 2-bromo-5-(trifluoromethyl)pyridine (7.45 g), tris(dibenzylideneacetone)dipalladium (1.37 g), 2,6-dimethoxy-2′ (dicyclohexylphosphino)biphenyl (2.46 g), cesium carbonate (29.3 g), dimethylformamide (100 mL) and water (25 ml) was stirred at 80° C. overnight under a nitrogen atmosphere. The reaction mixture was added to water, and the mixture was extracted with ethyl acetate. The extract was washed with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (13.6 g).

1. extractionthe mixture was extracted with ethyl acetate
2. washThe extract was washed with water and saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. customThe solvent was evaporated under reduced pressure
5. customthe residue was purified by silica gel column chromatography (hexane/ethyl acetate)

ORDレコード

ord-4f71309b11674efcb4c117bc129253f1

出典データセット

uspto-grants-2015_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09073864B2