反应详情

To a solution of 1-(3,4-dichloro-phenyl)-5-methyl-1H-imidazole-4-carboxylic acid ethyl ester (0.82 g, 2.7 mmol) in THF (27 ml) lithium aluminum hydride (0.21 g, 5.4 mmol) was added portionwise keeping T<10° C. The mixture was stirred in an ice-bath for 2 h, then 1 ml saturated aqueous Seignette salt solution was slowly added. After dilution with AcOEt (100 ml) the mixture was filtered, concentrated and chromatographed [silica, elution with gradient CH2Cl2 to 80% (CH2Cl2/MeOH=9:1)]. The title compound was obtained as a white crystalline solid (0.46 g, 66%). Mp. 174-175° C. (CH2Cl2/iPr2O), MS: m/e=256 (M+)

1. filtrationAfter dilution with AcOEt (100 ml) the mixture was filtered
2. concentrationconcentrated
3. customchromatographed
4. wash[silica, elution with gradient CH2Cl2 to 80% (CH2Cl2/MeOH=9:1)]