反应详情

温度

120 °C

A sealable vessel was charged with ethyl 7-bromoimidazo[1,2-a]pyridine-3-carboxylate (67 mg, 0.25 mmol), 4-((8-azabicyclo[3.2.1]octan-3-yloxy)methyl)-5-cyclopropyl-3-(2-(trifluoromethoxy)phenyl)isoxazole (I-1H) cesium carbonate (122 mg, 0.38 mmol), 1,4-dioxane (2 mL). The mixture was degassed (argon bubble, 10 min) and then tris(dibenzylideneacetone)dipalladium(0) (11 mg, 0.012 mmol), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (14 mg, 0.025 mmol) were added. The reaction flask was evacuated and backfilled with Ar three successive times, and then heated to 120° C. for 12 hours. The reaction mixture was cooled to RT, diluted with ethyl acetate (8 mL) and filtered through a CELITE® pad, the filtrate was washed with water (7 mL), dried over magnesium sulfate, concentrated, and chromatographed on silica using linear gradient, 0-100%, EtOAc in Hexanes) to give the desired product as a waxy solid.

1. customThe mixture was degassed
2. custom(argon bubble, 10 min)
3. customThe reaction flask was evacuated
4. temperatureThe reaction mixture was cooled to RT
5. additiondiluted with ethyl acetate (8 mL)
6. filtrationfiltered through a CELITE® pad
7. washthe filtrate was washed with water (7 mL)
8. dry with materialdried over magnesium sulfate
9. concentrationconcentrated
10. customchromatographed on silica using linear gradient, 0-100%, EtOAc in Hexanes)