反应详情

5-(4-Hydroxy-1-piperidyl)-6-fluoroquinaldine (3.7 g) was dissolved in a mixed solvent consisting of 100 ml of acetic acid and 10 ml of ethyl acetate, and 1 g of 5% palladium-carbon was added to the mixture which then was placed in a vitrified autoclave. The reaction mixture was stirred at room temperature under a hydrogen gas pressure of 5 kg/cm2 for 3 hours. After removing hydrogen gas the reaction mixture was taken out. After removing the catalyst, the content was concentrated to dryness, dissolved in 100 ml of chloroform and neutralized with 50 ml of an aqueous 5% sodium hydroxide solution. After separation and washing with 100 ml of water twice, the chloroform layer was dried and concentrated to dryness. To the residue were added 20 ml of hexane and 0.5 g activated carbon and the mixture was heated to dissolve. After removing activated carbon by filtration the hexane layer was cooled to precipitate crystals which then were collected to give 3.4 g of 5-(4-hydroxy-1-piperidyl)-6-fluoro-1,2,3,4-tetrahydroquinaldine.

1. additionwas added to the mixture which
2. customAfter removing hydrogen gas the reaction mixture
3. customAfter removing the catalyst
4. concentrationthe content was concentrated to dryness
5. dissolutiondissolved in 100 ml of chloroform and neutralized with 50 ml of an aqueous 5% sodium hydroxide solution
6. customAfter separation
7. washwashing with 100 ml of water twice
8. dry with materialthe chloroform layer was dried
9. concentrationconcentrated to dryness
10. additionTo the residue were added 20 ml of hexane and 0.5 g
11. temperaturethe mixture was heated to dissolve
12. customAfter removing activated carbon
13. filtrationby filtration the hexane layer
14. temperaturewas cooled
15. customto precipitate crystals which
16. customthen were collected