反应详情

53 mg of 3-(2-cyanophenyl)-5-(2-pyridyl)-1-phenyl-1,2-dihydropyridin-2-one was dissolved in 10 ml of ethanol containing 20% of water. 19 mg of hydroxylamine hydrochloride and 17 mg of sodium acetate were added thereto, followed by heating under reflux for 24 hours. Further, 19 mg of hydroxylamine hydrochloride and 17 mg of sodium acetate were added thereto, followed by heating under reflux for 36 hours. After cooling to room temperature, the mixture was evaporated, and the resulting crystals were washed with water, dried, and 50 mg of amidoxime compound was collected by filtration. 20 mg of the product was dissolved in 4 ml of toluene. 16 mg of acetic anhydride was added thereto, followed by heating under reflux for 96 hours. After cooling to room temperature, the mixture was neutralized with potassium carbonate under ice-cooling. After extracting with ethyl acetate, the extract was successively washed with water and brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated, and the residue was purified by silica gel chromatography (hexane/ethyl acetate system), to give 4 mg of the title compound.

1. temperatureby heating
2. temperatureunder reflux for 24 hours
3. temperatureby heating
4. temperatureunder reflux for 36 hours
5. customthe mixture was evaporated
6. washthe resulting crystals were washed with water
7. customdried
8. filtration50 mg of amidoxime compound was collected by filtration
9. dissolution20 mg of the product was dissolved in 4 ml of toluene
10. addition16 mg of acetic anhydride was added
11. temperatureby heating
12. temperatureunder reflux for 96 hours
13. temperatureAfter cooling to room temperature
14. temperaturecooling
15. extractionAfter extracting with ethyl acetate
16. washthe extract was successively washed with water and brine
17. dry with materialdried over anhydrous magnesium sulfate
18. customThe solvent was evaporated
19. customthe residue was purified by silica gel chromatography (hexane/ethyl acetate system)