反应详情

温度

80 °C

A mixture of 3-hydroxy-2-nitrotoluene (5 g), 2,2,2-trifluoroethyl methanesulfonate (8.7 g), anhydrous potassium carbonate (9 g) and N,N-dimethylformamide (40 ml) was heated, with stirring, on an oil bath at 80° C. for 4 hours, and then at 100° C. for 4 hours. The reaction solution was extracted with ethyl acetate-water. The organic layer was washed with water, followed by a dilute aqueous potassium carbonate solution and then saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate, and then filtered through NH silica gel, which was washed with ethyl acetate. The filtrate was concentrated under reduced pressure, and subjected to a silica-gel column chromatography with 5 to 10% ethyl acetate/hexane to yield the title compound (4.12 g).

1. temperaturewas heated
2. waitat 100° C. for 4 hours
3. extractionThe reaction solution was extracted with ethyl acetate-water
4. washThe organic layer was washed with water
5. dry with materialsaturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate
6. filtrationfiltered through NH silica gel, which
7. washwas washed with ethyl acetate
8. concentrationThe filtrate was concentrated under reduced pressure