反应详情

To a solution of 3.01 g of 5-[3,5-bis(trifluoromethyl)phenyl]-3-[4-(1-bromoethyl)phenyl]-5-trifluoromethyl-4,5-dihydroisoxazole in 10 mL of N,N-dimethylformamide, 1.26 g of potassium phthalimide was added and the resultant mixture was stirred at 80° C. for 3.5 hours. After the completion of the reaction, the reaction mixture was left to be cooled down to room temperature and 20 mL of water was added to the reaction mixture. The resultant mixture was extracted with ethyl acetate (70 mL×1). The organic phase was washed with water (20 mL×1) and then dehydrated and dried over saturated saline and anhydrous magnesium sulfate in this order and the solvent was distilled off under reduced pressure. The resultant residue was purified by silica gel column chromatography eluting with ethyl acetate-hexane (a gradient from 1:10 to 1:5) to obtain 2.80 g of the objective substance as a colorless resinoid.

1. customAfter the completion of the reaction
2. waitthe reaction mixture was left
3. extractionThe resultant mixture was extracted with ethyl acetate (70 mL×1)
4. washThe organic phase was washed with water (20 mL×1)
5. dry with materialdried over saturated saline and anhydrous magnesium sulfate in this order
6. distillationthe solvent was distilled off under reduced pressure
7. customThe resultant residue was purified by silica gel column chromatography
8. washeluting with ethyl acetate-hexane (a gradient from 1:10 to 1:5)
9. customto obtain 2.80 g of the objective substance as a colorless resinoid