反应详情

In a solution of 0.15 g of 4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazol-3-yl]-2-fluoro benzoic acid in 10 ml of dichloromethane, 0.3 ml of oxalyl chloride and 2 drops of N,N-dimethylformamide were added at room temperature, and stirred at the same temperature for 10 minutes. After the completion of the reaction, the solvent was distilled off under reduced pressure, the remaining white solid was dissolved in 10 ml of chloroform, and 0.3 ml of benzylamine and then 0.3 ml of triethylamine were added under cooling with ice, after the completion of the addition, continued to stir at room temperature for further 20 minutes. After the completion of the reaction, 40 ml of water was poured in the reaction mixture, and extracted with ethyl acetate (50 ml×1). The organic phase was 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 (1:2) to obtain 0.14 g of the aimed product as white crystal.

1. customAfter the completion of the reaction
2. distillationthe solvent was distilled off under reduced pressure
3. dissolutionthe remaining white solid was dissolved in 10 ml of chloroform
4. addition0.3 ml of benzylamine and then 0.3 ml of triethylamine were added
5. temperatureunder cooling with ice
6. additionafter the completion of the addition
7. stirringto stir at room temperature for further 20 minutes
8. customAfter the completion of the reaction, 40 ml of water
9. additionwas poured in the reaction mixture
10. extractionextracted with ethyl acetate (50 ml×1)
11. dry with materialdried over anhydrous sodium sulfate
12. distillationthe solvent was distilled off under reduced pressure
13. customThe residue was purified with silica gel column chromatography that