反应详情

A mixture of 2.800 g of 4-(4-methoxymethyl-phenyl)-1-trityl-1H-imidazole in 50 ml of TFA is stirred at room temperature for 3 hours. The reaction mixture is concentrated, taken up into ethyl acetate and the organic phase washed with sat. NaHCO3-solution and brine and dried over Na2SO4. Evaporation of the solvent gives a residue which is purified by flash chromatography on silica (40-63 μm particle size) with dichloromethane/methanol 93:7, yielding 1.169 g of 4-(4-methoxymethyl-phenyl)-1H-imidazole as a beige powder. Rt=2.906 min by HPLC on a nucleosil C18HD column with acetonitril+0.05% TFA/water+0.05% TFA, 20/80 to 100/0 over 6 min, 1.0 ml/min solvent flow. MS (API-ES, pos. scan): e/m=189 (M+1).

1. concentrationThe reaction mixture is concentrated
2. washthe organic phase washed with sat. NaHCO3-solution and brine
3. dry with materialdried over Na2SO4
4. customEvaporation of the solvent
5. customgives a residue which
6. customis purified by flash chromatography on silica (40-63 μm particle size) with dichloromethane/methanol 93:7