反应详情

1,1'-Carbonyldiimidazole (236 mg) was added to a stirred solution of 3,4-dichlorophenylacetic acid (314 mg) in dry dichloromethane (6 ml) at room temperature under nitrogen. The resulting solution was stirred at room temperature for 1 h and added dropwise to a cooled solution of 4-(phenylmethyl)-2-piperazinemethanol (300 mg) in dry dichloromethane (3 ml) and stirred at room temperature for 19 h. The reaction mixture was diluted with dichloromethane (5 ml) and washed with 2N sodium carbonate solution (3×10 ml). The organic layer was dried and evaporated to give an oil which was purified by flash column chromatography using gradient elution with dichloromethane:ethyl acetate (2:1), dichloromethane:ethyl acetate (1:1) and dichloromethane:methanol (9:1) to give the title compound as a solid (200 mg). m.p. 148°-150°.

1. stirringstirred at room temperature for 19 h
2. washwashed with 2N sodium carbonate solution (3×10 ml)
3. customThe organic layer was dried
4. customevaporated
5. customto give an oil which
6. customwas purified by flash column chromatography
7. washelution with dichloromethane:ethyl acetate (2:1), dichloromethane:ethyl acetate (1:1) and dichloromethane:methanol (9:1)