反应详情

温度

50 °C

To a suspension of 1-(3-bromo-4-chloro-benzenesulfonyl)-2,3,4,5-tetrahydro-1H-1-benzazepine, 2,4-dichloropyridine-5-boronic acid hydrate, tri-t-butylphosphonium tetrafluoroborate and tris(dibenzylideneacetone)dipalladium(0) in THF (0.73 mL) was added potassium hydroxide aqueous solution (0.05 g in 0.18 mL water). The suspension was bubbled with N2 for 5 min and then heated at 50° C. for 12 hrs. This mixture was cooled to it and concentrated. The residue was purified by silica gel column chromatography eluting with (hexanes/ethyl acetate, 20/1) to yield 1-[4-chloro-3-(4,6-dichloro-pyridin-3-yl)-benzenesulfonyl]-2,3,4,5-tetrahydro-1H-1-benzazepine 5-1 (9 mg, 8.7% yield). MS: 467 (M+H)+; tR=9.95 min (method 2).

1. customThe suspension was bubbled with N2 for 5 min
2. temperatureThis mixture was cooled to it
3. concentrationconcentrated
4. customThe residue was purified by silica gel column chromatography
5. washeluting with (hexanes/ethyl acetate, 20/1)