反应详情

温度

65 °C

Tetrakis(triphenylphosphine)palladium(0) (30 mg) was added to a solution of (5R)-1-(2,4-dimethoxybenzyl)-5-{(E)-2-(tributylstannyl)-2-[4-(trifluoromethyl)phenyl]ethenyl}pyrrolidin-2-one obtained in Reference Example 4-29 (184 mg), 3-(cyclopentyloxy)-6-iodo-2-methoxypyridine obtained in Reference Example 4-37 (169 mg), cesium fluoride (80 mg) and copper iodide (60 mg) in N,N-dimethylformamide (2 mL) in a nitrogen atmosphere, and the mixture was stirred at 65° C. for three hours. The reaction solution was left to cool, and then water and ethyl acetate were added, followed by filtration through celite. The filtrate was extracted with ethyl acetate. The organic layer was washed with water and brine and dried over anhydrous magnesium sulfate, after which the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=19:1→1:1) to give (5R)-5-{(E)-2-[5-(cyclopentyloxy)-6-methoxypyridin-2-yl]-2-[4-(trifluoromethyl)phenyl]ethenyl}-1-(2,4-dimethoxybenzyl)pyrrolidin-2-one as a light yellow oil (184 mg).

1. waitThe reaction solution was left
2. temperatureto cool
3. filtrationfollowed by filtration through celite
4. extractionThe filtrate was extracted with ethyl acetate
5. washThe organic layer was washed with water and brine
6. dry with materialdried over anhydrous magnesium sulfate
7. customafter which the solvent was evaporated under reduced pressure
8. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=19:1→1:1)