反应详情

温度

120 °C

A suspension of 5-chloro-2-nitrobenzonitrile (2.41 g), morpholin-3-one (2 g), cesium carbonate (6.45 g), tris(dibenzylideneacetone)dipalladium (120 mg) and 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (230 mg) in 30 ml dioxane was heated for 24 h at 120° C. The reaction mixture was cooled to 25° C., diluted with CH2Cl2 and filtered through decalite. The organic layer was washed with water and brine and purified by chromatography (silica gel, AcOEt) to yield 2-nitro-5-(3-oxo-morpholin-4-yl)-benzonitrile as a yellow solid (1.77 g). MH+=248.3

1. temperatureThe reaction mixture was cooled to 25° C.
2. filtrationfiltered through decalite
3. washThe organic layer was washed with water and brine
4. custompurified by chromatography (silica gel, AcOEt)