反应详情

13.8 g (50 mmol) of 3-(2,4-difluorophenyl)-6-trifluoromethyl-2H-pyran-2-one was dissolved in 150 ml of ethanol, and 5.5 g (70 mmol) of a 40% methylamine methanol solution was added, followed by stirring for 6 hours under heating and refluxing. The reaction solution was poured into ice water and extracted with ethyl acetate. After washing with 1N hydrochloric acid and water, the organic layer was dried over anhydrous magnesium sulfate. Ethyl acetate was distilled off under reduced pressure, and then, the obtained residue was purified by silica gel column chromatography to obtain 3.8 g (yield: 26%) of the desired product. Melting point: 123-124° C.

1. temperatureunder heating
2. temperaturerefluxing
3. extractionextracted with ethyl acetate
4. washAfter washing with 1N hydrochloric acid and water
5. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
6. distillationEthyl acetate was distilled off under reduced pressure
7. customthe obtained residue was purified by silica gel column chromatography