反应详情

1-[1-(1,2,2a,3,4,5-Hexahydroacenaphthylen-1-yl)piperidin-4-yl]-1,3-dihydro-2H-benzimidazol 2-one (1.00 g) was dissolved in DMF (30 ml), 60% sodium hydride (140 mg) was added, and the suspension was stirred for 1 hr. Then, N-(2-bromoethyl)phthalimide (818 mg) was added, and the mixture was stirred at 100° C. for 1 hr. The reaction mixture was cooled to room temperature, and poured into saturated aqueous ammonium chloride solution, and the mixture was extracted with ethyl acetate. The extract was washed with water and saturated brine, dried over magnesium sulfate, and concentrated. The obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give 2-{2-{3-[1-(1,2,2a,3,4,5-hexahydroacenaphthylen-1-yl)piperidin-4-yl]-1,3-dihydro-2-oxobenzimidazol-1-yl}ethyl}isoindole-1,3-dione.

1. stirringthe mixture was stirred at 100° C. for 1 hr
2. extractionthe mixture was extracted with ethyl acetate
3. washThe extract was washed with water and saturated brine
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated
6. customThe obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate)