反应详情

温度

90 °C

To a mixture of 1-(2-chloropyrimidin-4-yl)-3-ethyl-2-oxopyrrolidine-3-carbonitrile (100 mg) obtained in Step A of Example 2, 3-aminopyridine (45 mg), cesium carbonate (260 mg) and 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (37 mg) in tetrahydrofuran (2 mL) was added tris(dibenzylideneacetone)dipalladium(0) (37 mg), and the mixture was stirred overnight at 90° C. The insoluble substance was removed by filtration through Celite, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (NH, hexane/ethyl acetate), 4M hydrogen chloride in ethyl acetate (4 mL) was added thereto, and the mixture was stirred at room temperature for 5 min. The solvent was evaporated under reduced pressure, and the residue was recrystallized (ethyl acetate) to give the title compound (49 mg).

1. customThe insoluble substance was removed by filtration through Celite
2. customthe solvent was evaporated under reduced pressure
3. customThe residue was purified by silica gel column chromatography (NH, hexane/ethyl acetate), 4M hydrogen chloride in ethyl acetate (4 mL)
4. additionwas added
5. stirringthe mixture was stirred at room temperature for 5 min
6. customThe solvent was evaporated under reduced pressure
7. customthe residue was recrystallized (ethyl acetate)