反应详情

To a solution of 6-iodo[1,2,4]triazolo[4,3-α]pyridin-3(2H)-one (Intermediate 13, 360 mg, 1.379 mmol) in anhydrous dimethylformamide (DMF, 4 mL) was added sequentially cesium carbonate (1.35 g, 4.14 mmol) and iodomethane (0.52 mL), and the reaction mixture was stirred at room temperature overnight. The reaction mixture was then diluted with ethyl acetate, and the precipitated solids were removed by filtration. The filtrate was washed with saturated aqueous brine, dried (magnesium sulfate), and concentrated to dryness under reduced pressure. The residue was purified by preparative thin layer chromatography (silica gel, 3% methanol/dichloromethane) to afford the title compound. LC/MS 257.8 (M+1).

1. customthe precipitated solids were removed by filtration
2. washThe filtrate was washed with saturated aqueous brine
3. dry with materialdried (magnesium sulfate)
4. concentrationconcentrated to dryness under reduced pressure
5. customThe residue was purified by preparative thin layer chromatography (silica gel, 3% methanol/dichloromethane)