反应详情

A microwave vial was charged with 5-amino-2-methyl-thiazole-4-carboxylic acid (2-methyl-pyridin-4-yl)-amide (0.200 g, 0.806 mmol), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (Xantphos) (0.159 g, 0.275 mmol) and palladium dibenzylideneacetone (Pd2dba3)-chloroform complex (0.086 g, 0.083 mmol). Degassed dioxane (10 ml) was added, followed by 3-bromo-5-(trifluoromethyl)pyridine (0.223 g, 0.991 mmol) and cesium carbonate (0.527 g, 1.62 mmol) The vial was then irradiated in a microwave oven at 150° C. for 90 min. The mixture was diluted with THF and the solids filtered, washing with THF. The filtrate was evaporated and the residue purified by flash chromatography on silica gel with dichloromethane/methanol 100:0→90:10 gradient to yield the title compound (0.147 g, 46%) as an off-white solid, MS (ISP): m/e=394.0 (M+H+).

1. customwas then irradiated in a microwave oven at 150° C. for 90 min
2. filtrationthe solids filtered
3. washwashing with THF
4. customThe filtrate was evaporated
5. customthe residue purified by flash chromatography on silica gel with dichloromethane/methanol 100:0→90:10 gradient