反应详情

1-(Pyridin-3-yl)-1,3-dihydrobenzimidazole-2-one (0.2 g) was suspended in DMF (6 ml). Sodium hydride (55% in oil, 48 mg) was added under ice cooling, and the mixture was stirred at room temperature for 30 minutes. 1-Ethyl-7-(3-iodopropoxy)-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione (0.45 g) was added to the mixture. The mixture was stirred at room temperature for 3 hours. The reaction mixture was poured to ice water (100 ml), followed by extraction with ethyl acetate. The organic layer was dried over sodium sulfate and condensed under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate). The purified product was condensed under reduced pressure. A 0.5N-hydrogen chloride ethanol solution (1.9 ml) was added to an isopropyl alcohol solution of the residue. The mixture was condensed under reduced pressure. Ether was added to the residue. The generated insoluble matter was separated by filtration and dried to give the title compound (0.38 g) as a white powder.

1. stirringThe mixture was stirred at room temperature for 3 hours
2. extractionfollowed by extraction with ethyl acetate
3. dry with materialThe organic layer was dried over sodium sulfate and condensed under reduced pressure
4. customThe residue was purified by silica gel column chromatography (ethyl acetate)
5. customcondensed under reduced pressure
6. customcondensed under reduced pressure
7. customThe generated insoluble matter was separated by filtration
8. customdried