反应详情

To a solution of 4-(5-(3,6-dimethyl-2,4-dioxo-1-(3-trifluoromethylphenyl)-1,2,3,4-tetrahydropyrimidin-5-yl)-1H-pyrazol-1-yl)benzonitrile (prepared in Example 1) (205 mg) in acetonitrile (10 ml) were added lithium chloride (23 mg), ammonium hexanitrato cerate(IV) (498 mg) and acetic acid (2.5 ml) and the resulting mixture was stirred with heating under reflux for five hours. To the reaction mixture was 10% aqueous sodium thiosulfate solution (10 ml) followed by an addition of ethyl acetate (20 ml×2) such that the intended products were extracted into an organic layer. The organic layer was washed with saturated saline (20 ml), dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate) to afford 4-(4-chloro-5-(3,6-dimethyl-2,4-dioxo-1-(3-trifluoromethylphenyl)-1,2,3,4-tetrahydropyrimidin-5-yl)-1H-pyrazol-1-yl)benzonitrile (238 mg). UPLC/MS 486 (M+H)/1.13 min (measurement condition 9)

1. temperaturewith heating
2. temperatureunder reflux for five hours
3. extractionwere extracted into an organic layer
4. washThe organic layer was washed with saturated saline (20 ml)
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate)