反应详情

温度

80 °C

To a solution of 2.80 g of N-[1-[4-[5-[3,5-bis(trifluoromethyl)phenyl]-5-trifluoromethyl-4,5-dihydroisoxazole-3-yl]phenyl]ethyl]phthalimide in 10 mL of ethanol, 0.22 g of hydrazine monohydrate was added and the resultant reaction mixture was stirred at 80° C. for 2 hours. After the completion of the reaction, the mixture was cooled down to 0° C. and the deposited insoluble substance was filtered off, followed by cleaning the filtered substance with a small amount of chloroform. The filtrate and the resultant chloroform-cleaning liquid were combined and the solvent was distilled off under reduced pressure. The resultant residue was dissolved in 30 mL of ethyl acetate and the resultant solution was washed with water (10 mL×1). Subsequently, the washed solution was dehydrated and dried over saturated saline and anhydrous magnesium sulfate in this order, and the solvent was distilled off under reduced pressure to obtain 1.80 g of the objective substance as a yellow resinoid. This was used in the next process as it was without being further purified.

1. customthe resultant reaction mixture
2. customAfter the completion of the reaction
3. temperaturethe mixture was cooled down to 0° C.
4. filtrationthe deposited insoluble substance was filtered off
5. distillationthe solvent was distilled off under reduced pressure
6. dissolutionThe resultant residue was dissolved in 30 mL of ethyl acetate
7. washthe resultant solution was washed with water (10 mL×1)
8. dry with materialdried over saturated saline and anhydrous magnesium sulfate in this order
9. distillationthe solvent was distilled off under reduced pressure
10. customto obtain 1.80 g of the objective substance as a yellow resinoid