反应详情

A mixture of methyl 7-bromo-1-(3-methoxypropyl)-2,3-dihydro-1H-1-benzazepine-4-carboxylate (450 mg), 4-(2-propoxyethoxy)phenyl borate (313 mg) and potassium carbonate (351 mg) in toluene-ethanol-water (15-1.5-1.5 ml) was stirred at room temperature for 1 hour under argon atmosphere. To the reaction system was added tetrakistriphenylphosphinepalladium (73 mg), and the mixture was heated to reflux for 20 hours. After cooled to room temperature, the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine and dried with magnesium sulfate. After concentration under reduced pressure, the residue was separated and purified with column chromatography (ethyl acetate:hexane=1:4→1:2) to give methyl 1-(3-methoxypropyl)-7-[4-(2-propoxyethoxy)phenyl]-2,3-dihydro-1H-1-benzazepine-4-carboxylate (376 mg) as yellow oil.

1. temperaturethe mixture was heated
2. temperatureto reflux for 20 hours
3. temperatureAfter cooled to room temperature
4. extractionthe mixture was extracted with ethyl acetate
5. washThe organic layer was washed with water and saturated brine
6. dry with materialdried with magnesium sulfate
7. concentrationAfter concentration under reduced pressure
8. customthe residue was separated
9. custompurified with column chromatography (ethyl acetate:hexane=1:4→1:2)