反应详情

A mixture of 4-(6-bromo-[1,2,4]triazolo[1,5-a]pyridin-2-yl)morpholine (200 mg, 706 μmol), tert-butyl carbamate (99.3 mg, 848 μmol) and cesium carbonate (322 mg, 989 μmol) was purged several times with argon, then tris(dibenzylideneacetone)dipalladium(0) (12.9 mg, 14.1 μmol) and 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (16.3 mg, 28.3 μmol) were added and the mixture was purged with argon again, the vessel was then capped. The resulting mixture was refluxed for 20 hours. The mixture was evaporated to dryness under reduced pressure. Final purification by flash chromatography (20 g silicagel column using heptane/ethyl acetate 70-100% as eluent) afforded (2-morpholin-4-yl-[1,2,4]triazolo[1,5-a]pyridin-6-yl)-carbamic acid tert-butyl ester (46 mg, 20.4%) as yellow solid. Mp.: 166° C. MS: m/z=320.0 (M+H+).

1. customwas purged several times with argon
2. customthe mixture was purged with argon again
3. customthe vessel was then capped
4. temperatureThe resulting mixture was refluxed for 20 hours
5. customThe mixture was evaporated to dryness under reduced pressure
6. customFinal purification by flash chromatography (20 g silicagel column using heptane/ethyl acetate 70-100% as eluent)