反应详情

温度

120 °C

In a solution of 0.51 g of 4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazole-3-yl]-2-iodo benzoic acid methyl ester in 5 ml of N,N-dimethylformamide, 0.18 g of copper (I) iodide, 0.06 g of potassium fluoride and 0.27 g of chlorodifluoro acetic acid methyl ester were added, and stirred at 120° C. for 5 hours. After the completion of the reaction, the reaction mixture was left and cooled to room temperature, 50 ml of water was added and extracted with ethyl acetate (50 ml×2). The organic phase was washed with water, dehydrated with saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate, and then the solvent was distilled off under reduced pressure. The residue was purified with silica gel column chromatography that was eluated with ethyl acetate-hexane (1:4), and 0.45 g of the aimed product was obtained as pale yellow oily substance.

1. customAfter the completion of the reaction
2. waitthe reaction mixture was left
3. temperaturecooled to room temperature
4. extractionextracted with ethyl acetate (50 ml×2)
5. washThe organic phase was washed with water
6. dry with materialdried over anhydrous sodium sulfate
7. distillationthe solvent was distilled off under reduced pressure
8. customThe residue was purified with silica gel column chromatography that