反应详情

In a solution of 0.60 g of 4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazol-3-yl]-2-iodo benzoic acid synthesized similarly to Steps 1 to 4 of Synthetic Example 4 in 10 ml of methanol, 2 drops of concentrated sulfuric acid was added, and stirred under reflux with heat for 20 hours. After the completion of the reaction, the solvent was distilled off under reduced pressure, the residue was neutralized with 10 ml of saturated sodium hydrogen carbonate aqueous solution, then extracted with ethyl acetate (10 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 0.56 g of the aimed product was obtained as colorless oily substance.

1. temperatureunder reflux
2. temperaturewith heat for 20 hours
3. customAfter the completion of the reaction
4. distillationthe solvent was distilled off under reduced pressure
5. extractionextracted with ethyl acetate (10 ml×2)
6. washThe organic phase was washed with water
7. dry with materialdried over anhydrous sodium sulfate
8. distillationthe solvent was distilled off under reduced pressure
9. customThe residue was purified with silica gel column chromatography that