反应详情

20 Milliliters of 20% hydrous pyridine was added to 1.4 g of 4-[(2-acetylaminoethyl)iminomethylaminomethylamino]benzoic acid.hydrobromide, 1.0 g of 6-amidino-1-carbamoylmethyl-2-naphthol.hydrochloride, 884 mg of DCC and 43.6 mg of DMAP, followed by stirring for 2 hours under cooling with ice and 4 days at room temperature. The precipitate was filtered and the filtrate was added dropwise to 250 ml of a mixed liquid of ether and acetone (1:10) and this was stirred for 24 hours under cooling with ice. Then, the precipitate was collected by filtration. To this collected precipitate was added 7 ml of DMF to dissolve the precipitate with heating, and 1.46 ml of concentrated hydrochloric acid was added under cooling with ice and stirring. This solution was added dropwise to 400 ml of ether.acetone (1:20), followed by stirring for 1 hour under cooling with ice and then 24 hours under cooling with water. After the supernatant was decanted, 20 ml of DMF was again added to the residue to dissolve the residue with heating, and further 1.5 ml of concentrated hydrochloric acid was added under cooling with water and stirring. This solution was added dropwise to 400 ml of acetone, followed by stirring for 1 hour under cooling with ice and then 24 hours under cooling with water. Thereafter, the precipitate was collected by filtration to obtain a crude product.

1. filtrationThe precipitate was filtered
2. additionthe filtrate was added dropwise to 250 ml of a mixed liquid of ether and acetone (1:10)
3. stirringthis was stirred for 24 hours
4. temperatureunder cooling with ice
5. filtrationThen, the precipitate was collected by filtration
6. additionTo this collected precipitate was added 7 ml of DMF
7. dissolutionto dissolve the precipitate
8. temperaturewith heating
9. addition1.46 ml of concentrated hydrochloric acid was added
10. temperatureunder cooling with ice
11. stirringstirring
12. additionThis solution was added dropwise to 400 ml of ether
13. stirringby stirring for 1 hour
14. temperatureunder cooling with ice
15. temperature24 hours under cooling with water
16. customAfter the supernatant was decanted
17. addition20 ml of DMF was again added to the residue
18. dissolutionto dissolve the residue
19. temperaturewith heating
20. additionfurther 1.5 ml of concentrated hydrochloric acid was added
21. temperatureunder cooling with water
22. stirringstirring
23. additionThis solution was added dropwise to 400 ml of acetone
24. stirringby stirring for 1 hour
25. temperatureunder cooling with ice
26. temperature24 hours under cooling with water
27. filtrationThereafter, the precipitate was collected by filtration