反应详情

温度

70 °C

To a flask was added 7-bromo-5-fluoro-3-(3-fluoro-benzyl)-benzofuran (0.365 gm, 1.0 mmol), [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium (0.010 gm, 0.012 mmol), potassium phosphate (0.425 gm, 2.0 mmol), 1-(triisopropylsilyl)pyrrole-3-boronic acid (0.365 gm, 1.37 mmol), DME (12 ml) and water (2 ml). The mixture was evacuated and refilled with nitrogen while being sonicated. The mixture was heated in a microwave reactor for 15 minutes at 70° C., then for 15 minutes at 100° C., and then for 15 minutes at 130° C. The mixture was cooled, concentrated under reduced pressure, diluted with brine and extracted with ethyl acetate. The organic phase was absorbed onto a pad of silica gel that was rinsed with ethyl acetate/hexanes (250 ml, 1/9) and eluted to give 1-[5-fluoro-3-(3-fluoro-benzyl)-7-(1-triisopropylsilanyl-1H-pyrrol-3-yl)-benzofuran-2-yl]-ethanone (0.38 gm, 75% yield).

1. customThe mixture was evacuated
2. additionrefilled with nitrogen
3. customwhile being sonicated
4. waitfor 15 minutes at 130° C
5. temperatureThe mixture was cooled
6. concentrationconcentrated under reduced pressure
7. additiondiluted with brine
8. extractionextracted with ethyl acetate
9. customThe organic phase was absorbed onto a pad of silica gel that
10. washwas rinsed with ethyl acetate/hexanes (250 ml, 1/9)
11. washeluted