反应详情

Triethylamine(0.15 ml) was added to a acetonitrile solution (6 ml) of 1-ethyl-3,3,5-trimethyl-7-[(2-pyridin-3-yl-ethylamino)methyl]-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione(0.35 g). The mixture was cooled with ice. Benzenesulphonyl chloride(0.13 ml) was added, and the mixture was stirred at room temperature overnight. The reaction liquid was condensed under reduced pressure. Water was added to the residue, followed by extraction by ethyl acetate. The organic layer was dried over anhydrous sodium sulfate. After concentration under reduced pressure, the residue was purified by NH silica gel column chromatography (hexane: ethyl acetate=30:70). The purified product was condensed under reduced pressure, and the residue was recrystallized from the ethyl acetate-ether mixture to give the title compound(0.1 g) as a white powder.

1. temperatureThe mixture was cooled with ice
2. customThe reaction liquid
3. customcondensed under reduced pressure
4. extractionfollowed by extraction by ethyl acetate
5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
6. concentrationAfter concentration under reduced pressure
7. customthe residue was purified by NH silica gel column chromatography (hexane: ethyl acetate=30:70)
8. customcondensed under reduced pressure
9. customthe residue was recrystallized from the ethyl acetate-ether mixture