反应详情

温度

60 °C

4-Chloromethyl-1-(3,4-dichloro-phenyl)-1H-imidazole (1.31 g, 5.0 mmol) was dissolved in DMF (10 ml), 2-imidazolecarboxaldehyde (0.48 g, 5.0 mmol) and cesium carbonate (0.82 g, 2.5 mmol) was added and the resulting mixture was stirred at 60° C. for 12 h. After evaporation of the solvent the residue was dissolved in AcOEt and washed with H2O. The organic phase was dried (Na2SO4), concentrated and chromatographed [silica, elution with gradient CH2Cl2 to 100% (CH2Cl2/MeOH=9:1)] to obtain 0.98 g (61%) of the title compound as an off-white solid. Mp. 130-131° C. (CH2Cl2/iPr2O), MS: m/e=320 (M+).

1. customAfter evaporation of the solvent the residue
2. dissolutionwas dissolved in AcOEt
3. washwashed with H2O
4. dry with materialThe organic phase was dried (Na2SO4)
5. concentrationconcentrated
6. customchromatographed
7. wash[silica, elution with gradient CH2Cl2 to 100% (CH2Cl2/MeOH=9:1)]