反应详情

3 Milliliters of anhydrous pyridine was added to 418 mg of 4-aminoiminomethylaminobenzoic acid.methanesulfonate, 500 mg of 6-amidino-1-dimethylcarbamoylmethoxycarbonyl-2-naphthol.hydrochloride, 400 mg of DCC and 18 mg of DMAP, followed by stirring for 2 hours under cooling with ice and then 24 hours at room temperature. Then, the precipitate was collected by filtration and dissolved with addition of 20 ml of warm DMF, followed by stirring for 1 hour under cooling with ice. The precipitate was filtered and the filtrate was added dropwise to 400 ml of ether, followed by stirring for 24 hours under cooling with ice. The precipitate was collected by filtration and dissolved with addition of 20 ml of water, and the solution was added dropwise to 100 ml of aqueous sodium bicarbonate solution, followed by stirring for 2 hours under cooling with ice. Then, the precipitate was collected by filtration and washed with small amounts of water and acetone. This was added to a solution comprising 20 ml of DMF and 0.36 ml of methanesulfonic acid. The resulting solution was added dropwise to 450 ml of acetone, followed by stirring for 24 hours under cooling with ice. Then, the precipitate was collected by filtration to obtain 312.5 mg of the desired product.

1. temperatureunder cooling with ice
2. custom24 hours
3. customat room temperature
4. filtrationThen, the precipitate was collected by filtration
5. dissolutiondissolved with addition of 20 ml of warm DMF
6. stirringby stirring for 1 hour
7. temperatureunder cooling with ice
8. filtrationThe precipitate was filtered
9. additionthe filtrate was added dropwise to 400 ml of ether
10. stirringby stirring for 24 hours
11. temperatureunder cooling with ice
12. filtrationThe precipitate was collected by filtration
13. dissolutiondissolved with addition of 20 ml of water
14. additionthe solution was added dropwise to 100 ml of aqueous sodium bicarbonate solution
15. stirringby stirring for 2 hours
16. temperatureunder cooling with ice
17. filtrationThen, the precipitate was collected by filtration
18. washwashed with small amounts of water and acetone
19. additionThis was added to a solution
20. additionThe resulting solution was added dropwise to 450 ml of acetone
21. stirringby stirring for 24 hours
22. temperatureunder cooling with ice
23. filtrationThen, the precipitate was collected by filtration