反应详情

温度

150 °C

To a solution of 5-(4-trifluoromethoxyphenyl)-[1,3,4]oxathiazol-2-one (0.74 g, 2.81 mmol) in n-dodecane (0.50 ml) was added ethyl cyanoformate (1.10 ml, 11.24 mmol). The resulting reaction mixture was refluxed for 24 h at 150° C. After the completion of the reaction (TLC monitoring), added ice-cold water and extracted with ethyl acetate (3×50 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, 2% EtOAc-Hexane) to get the product (0.11 g, 12%).

1. customThe resulting reaction mixture
2. customAfter the completion of the reaction (TLC monitoring)
3. additionadded ice-cold water
4. extractionextracted with ethyl acetate (3×50 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, 2% EtOAc-Hexane)