反应详情

温度

130 °C

To a mixture of 4-chloro-N-(1-methyl-1H-pyrazol-4-yl)pyrimidin-2-amine (150 mg) obtained in Step C of Example 1, 3,3-diethylpyrrolidin-2-one (110 mg), cesium carbonate (700 mg) and 2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (90 mg) in tetrahydrofuran (5 mL) was added tris(dibenzylideneacetone)dipalladium(0) (130 mg), and the mixture was stirred in a microwave reactor at 130° C. for 1.5 hr. 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 (hexane/ethyl acetate), to a solution of the residue in ethanol (5 mL) was added 12M hydrogen chloride ethanol solution (1 mL), and the mixture was stirred at room temperature for 5 min. The solvent was evaporated under reduced pressure, and the obtained crude crystals were recrystallized (ethanol/ethyl acetate) to give the title compound (76 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 (hexane/ethyl acetate), to a solution of the residue in ethanol (5 mL)
4. additionwas added 12M hydrogen chloride ethanol solution (1 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 (ethanol/ethyl acetate)