反应详情

1-[5-bromo-2-nitro-4-(trifluoromethyl)phenyl]-1H-imidazole (15.50 g, 0.0461 mol) is stirred with SnCl2.2H2O (51.77 g, 0.2274 mol) in ethanol (78 mL) at 80° C. for 2 hours. After cooling down to room temperature, the mixture is concentrated and partitioned between water (200 mL) and ethyl acetate (250 mL). Sodium hydrogencarbonate powder is added to adjust the pH to 8. The milky suspension is filtrated, the cake is washed with ethyl acetate and the combined organic phases are washed with water and dried over sodium sulfate. Concentration affords the title compound as a pale yellow solid (12.70 g, 90.0%)

1. concentrationthe mixture is concentrated
2. custompartitioned between water (200 mL) and ethyl acetate (250 mL)
3. additionSodium hydrogencarbonate powder is added
4. filtrationThe milky suspension is filtrated
5. washthe cake is washed with ethyl acetate
6. washthe combined organic phases are washed with water
7. dry with materialdried over sodium sulfate
8. concentrationConcentration