反应详情

温度

25 °C

To a solution of 5-bromomethyl-3-(4-trifluoromethoxyphenyl)-[1,2,4]thiadiazole (0.11 g, 0.32 mmol) in DMF (5 ml) was added 2,6-difluoro-3-hydroxybenzamide (0.056 g, 0.32 mmol) and potassium carbonate (0.16 g, 1.13 mmol). The reaction mixture was stirred at 25° C. for 12 h under nitrogen atmosphere. After the completion of the reaction (TLC monitoring), the reaction mixture was evaporated to dryness under vacuum, added 30 ml water and extracted with ethyl acetate (3×20 ml). The combined organic layer was dried over Na2SO4, filtered and concentrated under vacuum. The crude residue was purified over silica gel (100-200 M, 50% EtOAc-Hexane) to get the desired product (0.013 g, 9%).

1. customAfter the completion of the reaction (TLC monitoring)
2. customthe reaction mixture was evaporated to dryness under vacuum
3. additionadded 30 ml water
4. extractionextracted with ethyl acetate (3×20 ml)
5. dry with materialThe combined organic layer was dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated under vacuum
8. customThe crude residue was purified over silica gel (100-200 M, 50% EtOAc-Hexane)