反应详情

温度

90 °C

To a solution of tris(dibenzylideneacetone)dipalladium(0) (835 mg) and 4,5′-bis(diphenylphosphino)-9,9′-dimethylxanthene (1.06 g) in 1,4-dioxane (125 mL), 2-(5-(2-chloro-4-(pyrrolidin-1-yl)pyrimidin-5-yl)-4-pentyn-1-yl)isoindoline-1,3-dione (H2, 3.60 g), 4-aminobenzonitrile (2.69 g) and cesium carbonate (8.90 g) were added at room temperature under a nitrogen atmosphere, and the mixture was stirred at 90° C. for 7 hours. The reaction mixture was cooled to room temperature, and then ethyl acetate was added to the reaction mixture. The insoluble matter was removed by filtration through Cerite, and then the solvent was evaporated under reduced pressure. To the obtained residue, water was added. The solid matter was taken by filtration, and washed with water to obtain 4-((5-(5-(1,3-dioxoisoindolin-2-yl)-1-pentyn-1-yl)-4-(pyrrolidin-1-yl)pyrimidin-2-yl)amino)benzonitrile (H3).

1. temperatureThe reaction mixture was cooled to room temperature
2. customThe insoluble matter was removed by filtration through Cerite
3. customthe solvent was evaporated under reduced pressure
4. additionTo the obtained residue, water was added
5. filtrationThe solid matter was taken by filtration
6. washwashed with water