反应详情

温度

100 °C

To a solution of 5-bromo-1-methyl-1H-indazole (76 mg, 0.36 mmol) in 1,4-dioxane (5 mL) was added tetrahydropyrimidin-2(1H)-one (Aldrich, 216 mg, 2.16 mmol), followed by Pd2(dba)3 (16 mg, 0.02 mmol), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (31 mg, 0.06 mmol) and cesium carbonate (176 mg, 0.54 mmol). The reaction mixture was degassed with nitrogen and heated at 100° C. for 16 hours. The mixture was diluted with ethyl acetate, washed with water and brine, and dried over Na2SO4 and filtered. Concentration and purification by flash column chromatography (hexanes/EtOAc) yielded 1-(1-methyl-1H-indazol-5-yl)tetrahydropyrimidin-2(1H)-one. LCMS-ESI+: calc'd for C12H14N4O: 231.2 (M+H+); Found: 231.2 (M+H+).

1. customThe reaction mixture was degassed with nitrogen
2. additionThe mixture was diluted with ethyl acetate
3. washwashed with water and brine
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationConcentration and purification by flash column chromatography (hexanes/EtOAc)