反応 #75810

反応方程式

sodium hydrogencarbonate

sodium chloride

1-(piperidin-4-yl)-1,3-dihydro-2H-benzimidazol-2-one

1-(diphenylmethyl)azetidin-2-one

sodium cyanoborohydride

→

1-[1-[1-(diphenylmethyl)azetidin-3-yl]piperidin-4-yl]-1,3-dihydro-2H-benzimidazol-2-one

収率 133.1%

溶媒

methanol

反応条件

後処理

1. 1
   その他The reaction liquid
2. 2
   workup.ADDITIONhad been added
3. 3
   抽出extracted with ethyl acetate
4. 4
   洗浄The extract was washed with saturated brine
5. 5
   乾燥dried over sodium sulfate
6. 6
   濃縮concentrated
7. 7
   その他Thus obtained residue was purified by silica gel column chromatography (chloroform, chloroform/methanol=50/1)

実験手順

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.

出典