反应详情

Benzimidazole-5-carboxylic acid (1 mMol, 162 mg) was dissolved in 5 mL dry DMF and reacted with 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride for 15 minutes. 1-(3,4-dichlorophenyl)-piperazine, 1 mMol (231 mg) was added followed by 10 mg DMAP. The mixture was stirred for 20 h at room temperature. The reaction mixture was poured into water and extracted with methylene chloride (3×50 mL). The extracts were combined, washed with brine, water and dried over MgSO4. After evaporation of the solvent, the residue was chromatographed on silica gel with chloroform-methanol (0-5% methanol, gradient). Evaporation of the desired fractions gave 150 mg (40%) of the title compound; MS (ESI) m/e 375 (M+).

1. extractionextracted with methylene chloride (3×50 mL)
2. washwashed with brine, water
3. dry with materialdried over MgSO4
4. customAfter evaporation of the solvent
5. customthe residue was chromatographed on silica gel with chloroform-methanol (0-5% methanol, gradient)
6. customEvaporation of the desired fractions