反应详情

温度

80 °C

To a solution of (3R)-1-(2-chloropyrimidin-4-yl)-3-ethyl-2-oxopyrrolidine-3-carbonitrile (130 mg) obtained in Step A of Example 8, 2-(5-aminopyridin-2-yl)acetamide (78 mg) obtained in Step D of Example 363, cesium carbonate (340 mg) and 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (48 mg) in tetrahydrofuran (5.0 mL) was added tris(dibenzylideneacetone)dipalladium(0) (48 mg), and the mixture was stirred overnight at 80° C. under argon atmosphere. 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, ethyl acetate/methanol). To a solution of the residue (200 mg) in ethanol (2.0 mL) was added 1 M hydrochloric acid (0.55 mL), the mixture was stirred at room temperature for 5 min, and the solvent was evaporated under reduced pressure. The obtained crude crystals were recrystallized (diisopropyl ether/ethanol) to give the title compound (42 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, ethyl acetate/methanol)
4. additionTo a solution of the residue (200 mg) in ethanol (2.0 mL) was added 1 M hydrochloric acid (0.55 mL)
5. stirringthe mixture was stirred at room temperature for 5 min
6. customthe solvent was evaporated under reduced pressure
7. customThe obtained crude crystals
8. customwere recrystallized (diisopropyl ether/ethanol)