反应详情

In a solution of 0.29 g of 2,2,2-trifluoroethylamine and 0.37 g of triethylamine in 20 ml of chloroform, 1.81 g of the crude 4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazol-3-yl]benzoic acid chloride dissolved in 10 ml of chloroform was added dropwise with cooling with ice and with stirring. After the completion of addition dropwise, the mixture was continued to stir at room temperature further for 30 minutes. After the completion of the reaction, the reaction mixture was poured in 100 ml of water, and extracted with chloroform (20 ml×3), the organic phase was washed with water, dehydrated with saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate, and passed through a glass filter packed with silica gel, and then the solvent was distilled off under reduced pressure. The residual solid was washed with hexane to obtain 1.05 g of the aimed product as white crystal.

1. additionwas added dropwise
2. temperaturewith cooling with ice
3. additionAfter the completion of addition dropwise
4. stirringto stir at room temperature further for 30 minutes
5. customAfter the completion of the reaction
6. extractionextracted with chloroform (20 ml×3)
7. washthe organic phase was washed with water
8. dry with materialdried over anhydrous sodium sulfate
9. filtrationfilter
10. distillationthe solvent was distilled off under reduced pressure
11. washThe residual solid was washed with hexane