反应详情

温度

85 °C

To a mixture of (3S,5S)-3-cyclopropyl-5-methyl-2-oxopyrrolidine-3-carbonitrile (150 mg) obtained in Step B of Example 358, 2-(4-((4-chloropyrimidin-2-yl)amino)-1H-pyrazol-1-yl)-2-methylpropan-1-ol (200 mg) obtained in Step E of Example 347, potassium carbonate (210 mg) and 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (26 mg) in toluene (2.0 mL) was added tris(dibenzylideneacetone)dipalladium(0) (14 mg), and the mixture was stirred overnight at 85° 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), and to a solution of the residue (200 mg) in ethanol (2.0 mL) was added 1 M hydrochloric acid (0.51 mL). The reaction mixture was concentrated under reduced pressure, and the residue was recrystallized (diisopropyl ether/ethyl acetate) to give the title compound (65 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)
4. additionto a solution of the residue (200 mg) in ethanol (2.0 mL) was added 1 M hydrochloric acid (0.51 mL)
5. concentrationThe reaction mixture was concentrated under reduced pressure
6. customthe residue was recrystallized (diisopropyl ether/ethyl acetate)