反应详情

In THF (5.2 ml) was dissolved 7-(4-ethylthiophenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (260 mg). To the mixture were added at room temperature thionyl chloride (0.06 ml) and DMF (one drop), and the mixture was stirred at room temperature for 1 hour. The reaction mixture was added dropwise to a solution of 4-[[N-(3-ethoxypropyl)-N-methylamino]methyl]aniline (0.58 ml) in THF (5.2 ml), and the mixture was stirred at room temperature for 2 hours. The reaction mixture 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 7-(4-ethylthiophenyl)-N-[4-[[N-(3-ethoxypropyl)-N-methylamino]methyl]phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide (Compound 82) (115 mg).

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