反应详情

To a stirred suspension of 2-[2-(3-chloro-phenyl)-2-methoxy-ethyl]-1-trityl-1H-imidazole (0.24 g) at room temperature in ethanol (2 ml) under an argon atmosphere was added 2 N HCl (3 ml). The mixture was heated to reflux. Stirring was continued for 3 hours. The mixture was cooled to room temperature and concentrated to leave a light yellow solid. This was taken up in H2O and brought to pH=12 by the addition of 4 N NaOH. The product was extracted with CH2Cl2/methanol 4:1. The combined organics were dried over MgSO4, filtered and concentrated. The crude product was purified by column chromatography (silica gel; gradient:CH2Cl2→CH2Cl2/methanol 9:1) to give 2-[2-(3-chloro-phenyl)-2-methoxy-ethyl]-1H-imidazole (0.11 mg) as light yellow gum. MS 237.1 ([M+H]+)

1. temperatureThe mixture was heated to reflux
2. concentrationconcentrated
3. customto leave a light yellow solid
4. extractionThe product was extracted with CH2Cl2/methanol 4:1
5. dry with materialThe combined organics were dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. customThe crude product was purified by column chromatography (silica gel; gradient:CH2Cl2→CH2Cl2/methanol 9:1)