反应详情

5.0 Grams of 6-(1-oxo-4-chlorobutyl)-3,4-dihydrocarbostyril and 3.5 g of sodium iodine were mixed in 100 ml of acetone and the mixture was stirred at 40°-50° C. for 5 hours. Then 80 ml of dimethylformamide was added to the mixture and acetone was removed from the mixture by distillation under reduced pressure. To this reaction mixture, 5.0 g of 4-phenylpiperazine and 5 g of triethylamine were added and stirred at 70°-80° C. for 6 hours. The reaction mixture was concentrated under a reduced pressure and 50 ml of 5%-sodium hydrogencarbonate solution was stirred to effect crystallization. Crude crystals thus formed were collected by filtration and washed with water and dried. Then the dried crude crystals were dispersed in 80 ml of chloroform and stirred at a room temperature for 1 hour. Insoluble matters in the chloroform solution were removed from the solution and chloroform was removed by distillation to obtain the residue. To the residue thus obtained was added 50 ml of methanol and 10 ml of concentrated hydrochloric acid and mixture was concentrated under a reduced pressure to dryness. To the residue thus obtained was added 50 ml of acetone and stirred to obtain crude crystals. The crude crystals were collected by filtration and washed with acetone and recrystallized from ethanol-water to obtain 5.7 g of 6-[1-oxo-4-(4-phenyl-1-piperazinyl)butyl]-3,4-dihydrocarbostyril monohydrochloride in yellowish powdery crystals.

1. customwas removed from the mixture by distillation under reduced pressure
2. additionTo this reaction mixture, 5.0 g of 4-phenylpiperazine and 5 g of triethylamine were added
3. stirringstirred at 70°-80° C. for 6 hours
4. concentrationThe reaction mixture was concentrated under a reduced pressure and 50 ml of 5%-sodium hydrogencarbonate solution
5. stirringwas stirred
6. customcrystallization
7. customCrude crystals thus formed
8. filtrationwere collected by filtration
9. washwashed with water
10. customdried
11. customThen the dried crude crystals
12. additionwere dispersed in 80 ml of chloroform
13. stirringstirred at a room temperature for 1 hour
14. customInsoluble matters in the chloroform solution were removed from the solution and chloroform
15. customwas removed by distillation
16. customto obtain the residue
17. customTo the residue thus obtained
18. concentrationwas concentrated under a reduced pressure to dryness
19. customTo the residue thus obtained
20. stirringstirred
21. customto obtain crude crystals
22. filtrationThe crude crystals were collected by filtration
23. washwashed with acetone
24. customrecrystallized from ethanol-water