反应详情

温度

25 °C

To a solution of 5-bromomethyl-3-(4-chlorophenyl)-[1,2,4]thiadiazole (0.24 g, 0.82 mmol) in DMF (7 ml) was added 2,6-difluoro-3-hydroxybenzonitrile (0.12 g, 0.74 mmol) and potassium carbonate (0.39 g, 2.90 mmol). The reaction mixture was stirred at 25° C. for 2 h under nitrogen atmosphere. After the completion of the reaction (TLC monitoring), the reaction mixture was evaporated to dryness under vacuum, added 50 ml water and extracted with ethyl acetate (3×40 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, 15% EtOAc-Hexane) to get the desired product (0.30 g, 73%).

1. customAfter the completion of the reaction (TLC monitoring)
2. customthe reaction mixture was evaporated to dryness under vacuum
3. additionadded 50 ml water
4. extractionextracted with ethyl acetate (3×40 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, 15% EtOAc-Hexane)