反应详情

In a solution of 0.37 g of glycine amide hydrochloride and 0.71 g of pyridine in 20 ml of dichloromethane, a solution of 1.31 g of 4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazol-3-yl]-2-methylbenzoyl chloride synthesized in Step 3 of Synthetic Example 29 in 10 ml of dichloromethane was added dropwise with stirring under ice cooling, after the completion of the addition, stirred at room temperature for 3 hours, then 3.00 g of triethyl amine was added in the reaction mixture, and continued to stir at the same temperature further for 30 minutes. After the completion of the reaction, the solvent was distilled off under reduced pressure, 50 ml of ethyl acetate and 50 ml of water were added in the residue, and the organic phase was collected, and the aqueous phase was further extracted with ethyl acetate (50 ml×2). The organic phases together were dehydrated and dried with saturated sodium chloride aqueous solution and anhydrous sodium sulfate in that order, and the solvent was distilled off under reduced pressure, the residual solid was washed with hexane to obtain 1.24 g of the aimed product as white crystal.

1. additionafter the completion of the addition
2. stirringstirred at room temperature for 3 hours
3. stirringto stir at the same temperature further for 30 minutes
4. customAfter the completion of the reaction
5. distillationthe solvent was distilled off under reduced pressure, 50 ml of ethyl acetate and 50 ml of water
6. additionwere added in the residue
7. customthe organic phase was collected
8. extractionthe aqueous phase was further extracted with ethyl acetate (50 ml×2)
9. dry with materialdried with saturated sodium chloride aqueous solution and anhydrous sodium sulfate in that order
10. distillationthe solvent was distilled off under reduced pressure
11. washthe residual solid was washed with hexane