反应详情

温度

80 °C

tert-Butyl 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole-1-carboxylate (216 mg), tris(dibenzylideneacetone)dipalladium(0) (33.7 mg), tri(2-furyl)phosphine (51.5 mg) and cesium carbonate (239 mg) were added to a solution of (5R)-5-[(E)-2-(5-bromo-6-methoxypyridin-2-yl)-2-(4-chlorophenyl)ethenyl]-1-(2,4-dimethoxybenzyl)pyrrolidin-2-one obtained in Reference Example 4-43 (200 mg) in 1,4-dioxane (3 mL)-water (1 mL), and the mixture was stirred at an external temperature for 80° C. for three hours. The reaction solution was left to cool, diluted with ethyl acetate and filtered through celite. The filtrate was washed with brine and dried over sodium sulfate. After filtration, the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1→7:3) to give (5R)-5-{(E)-2-(4-chlorophenyl)-2-[6-methoxy-5-(1H-pyrazol-4-yl)pyridin-2-yl]ethenyl}-1-(2,4-dimethoxybenzyl)pyrrolidin-2-one as a colorless oil (125 mg, 63%).

1. waitThe reaction solution was left
2. temperatureto cool
3. filtrationfiltered through celite
4. washThe filtrate was washed with brine
5. dry with materialdried over sodium sulfate
6. filtrationAfter filtration
7. customthe solvent was evaporated under reduced pressure
8. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1→7:3)