反应详情

温度

100 °C

Cesium carbonate (0.154 g, 0.473 mmol), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (0.027 g, 0.047 mmol), Pd2(dba)3 (0.0217 g, 0.023 mmol), 3-methoxy-phenylamine (0.038 g, 0.308 mmol) were added under argon to a solution of 2-[2-(1,3-Dioxo-1,3-dihydro-isoindol-2-yl)-pyrimidin-4-yl]-3-iodo-1-methyl-4-oxo-1,4,6,7-tetrahydro-pyrrolo[3,2-c]pyridine-5-carboxylic acid tert-butyl ester (0.142 mg, 0.237 mmol) in dry dioxane (4.0 ml) and the reaction mixture was stirred at 100° C. for 24 h under argon atmosphere. The solvent was removed under vacuum, the residue was taken up into DCM (5.0 ml), filtered, and the organic layer was washed with purite water (1×5.0 ml), dried over Na2SO4. The filtrate was purified over silica, using DCM/MeOH (9.5:0.5) as eluent, affording 2-(2-Amino-pyrimidin-4-yl)-3-(3-methoxy-phenylamino)-1-methyl-4-oxo-1,4,6,7-tetrahydro-pyrrolo[3,2-c]pyridine-5-carboxylic acid tert-butyl ester (0.025 g, 0.053 mmol, 23%).

1. customThe solvent was removed under vacuum
2. filtrationfiltered
3. washthe organic layer was washed with purite water (1×5.0 ml)
4. dry with materialdried over Na2SO4
5. customThe filtrate was purified over silica