反应详情

In 7 ml of methanol, 217 mg of 1-(piperidin-4-yl)-1,3-dihydro-2H-benzimidazol-2-one, 300 mg of 1-(diphenylmethyl)azetidin-2-one, 94 mg of sodium cyanoborohydride and 102 mg of zinc chloride were dissolved and stirred overnight. The reaction liquid was added to a saturated aqueous solution of sodium hydrogencarbonate to which sodium chloride had been added, and extracted with ethyl acetate. The extract was washed with saturated brine, dried over sodium sulfate and concentrated. Thus obtained residue was purified by silica gel column chromatography (chloroform, chloroform/methanol=50/1) to provide 583 mg of crude 1-[1-[1-(diphenylmethyl)azetidin-3-yl]piperidin-4-yl]-1,3-dihydro-2H-benzimidazol-2-one.

1. customThe reaction liquid
2. additionhad been added
3. extractionextracted with ethyl acetate
4. washThe extract was washed with saturated brine
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated
7. customThus obtained residue was purified by silica gel column chromatography (chloroform, chloroform/methanol=50/1)