反应详情

A mixture of 72 mg of 3-thenoic acid, 187 mg of 1-[1-(piperidin-4-yl)piperidin-4-yl]-1,3-dihydro-2H-benzimidazol-2-one dihydrochloride, 110 mg of ethyl 3-(dimethylamino)propylcarbodiimide, 110 mg of 1-hydroxy-1,2,3-benzotriazole, 300 mg of triethylamine, 10 ml of CHCl3, and 10 ml of tert-butyl alcohol was stirred for 17 h. The reaction mixture was partitionized between chloroform and aqueous NaHCO3. The organic layer was washed with aqueous NaHCO3, dried over anhydrous Na2SO4, and concentrated. The residue was purified on SiO2 chromatography (chloroform/methanol=30:1-20:1) to afford 180 mg of 1-[1-[1-(3-thenoyl)piperidin-4-yl]piperidin-4-yl]-1,3-dihydro-2H-benzimidazol-2-one as a colorless amorphous.

1. washThe organic layer was washed with aqueous NaHCO3
2. dry with materialdried over anhydrous Na2SO4
3. concentrationconcentrated
4. customThe residue was purified on SiO2 chromatography (chloroform/methanol=30:1-20:1)