反应详情

To 7-bromo-N-[4-[[N-methyl-N-(tetrahydropyran-4-yl)amino]methyl]phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide (300 mg) was added toluene/ethanol/water (20/1/1, 13.8 ml) and then were added 2-propoxyphenyl borate (125 mg) and potassium carbonate (175 mg), and the mixture was stirred at room temperature for 30 minutes. To the mixture was added tetrakistriphenylphosphinepalladium (27 mg), and the mixture was refluxed at 100° C. for 8 hours and cooled to room temperature. The mixture was added to water, and the mixture was extracted with ethyl acetate, washed with saturated brine and dried with magnesium sulfate. Under reduced pressure, the solvent was evaporated, and the residue was purified with silica gel column chromatography (ethyl acetate/ethanol=3/1) and recrystallized from ethanol to give N-[4-[[N-methyl-N-(tetrahydropyran-4-yl)amino]methyl]phenyl]-7-(2-propoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide (Compound 113) (46 mg).

1. temperaturethe mixture was refluxed at 100° C. for 8 hours
2. temperaturecooled to room temperature
3. extractionthe mixture was extracted with ethyl acetate
4. washwashed with saturated brine
5. dry with materialdried with magnesium sulfate
6. customUnder reduced pressure, the solvent was evaporated
7. customthe residue was purified with silica gel column chromatography (ethyl acetate/ethanol=3/1)
8. customrecrystallized from ethanol