反应详情

温度

85 °C

1 g of 10% palladium-on-charcoal and 100 mL of water are introduced into a 500 mL three-necked flask. A solution, prepared beforehand, of 13.3 g of N-(1-benzylpiperidin-4-yl)-7-methoxy-4-(4-methoxyphenyl)phthalazin-1-amine (compound 7) in 50 mL of ethanol and 4.4 mL of formic acid is added dropwise over 1 hour, to this mixture with stirring at 85° C. The reaction mixture is stirred at reflux for 2 hours. After cooling to room temperature, the ethanol is evaporated off under reduced pressure. The mixture is then basified to pH 12 with 2N sodium hydroxide solution and is then extracted with dichloromethane. The organic phase is washed with saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate and then evaporated under reduced pressure. The yellow oil obtained is concreted in diisopropyl ether to give a white solid. After filtration and drying under vacuum in the presence of phosphorus pentoxide, 10.29 g of 7-methoxy-4-(4-methoxyphenyl)-N-(piperidin-4-yl)-phthalazin-1-amine are obtained (97% yield).

1. customA solution, prepared beforehand
2. stirringThe reaction mixture is stirred
3. temperatureat reflux for 2 hours
4. temperatureAfter cooling to room temperature
5. customthe ethanol is evaporated off under reduced pressure
6. extractionis then extracted with dichloromethane
7. washThe organic phase is washed with saturated aqueous sodium chloride solution
8. dry with materialdried over anhydrous sodium sulfate
9. customevaporated under reduced pressure
10. customThe yellow oil obtained
11. customto give a white solid
12. filtrationAfter filtration
13. dry with materialdrying under vacuum in the presence of phosphorus pentoxide, 10.29 g of 7-methoxy-4-(4-methoxyphenyl)-N-(piperidin-4-yl)-phthalazin-1-amine
14. customare obtained (97% yield)