反应详情

90 Milliliters of 20% hydrous pyridine was added to 5.08 g of 4-aminoiminomethylaminobenzoic acid.methanesulfonate, 4.5 g of 6-amidino-1-(2-carbamoylvinyl)-2-naphthol.hydrochloride, 6.34 g of DCC and 80 mg of DMAP, followed by stirring for 2 hours under cooling with ice and then 48 hours at room temperature. Then, the precipitate was collected by filtration and washed twice with 160 ml of warm 20% hydrous pyridine. The above-obtained reaction filtrate and the warm hydrous pyridine wash liquid were combined and the resulting solution was added to 1 liter of acetone, followed by stirring for 24 hours under cooling with ice. The precipitate was collected by filtration and thereto was added 70 ml of warm DMF to dissolve the precipitate. Then, 0.5 g of active carbon was added, followed by stirring for 30 minutes at room temperature. Insoluble matter was filtered and 8.4 ml of concentrated hydrochloric acid was added to the filtrate. The resulting solution was added dropwise to 600 ml of acetone, followed by stirring for 24 hours under cooling with ice. Then, the precipitate was collected by filtration to obtain 6.8 g of the desired product.

1. temperatureunder cooling with ice
2. custom48 hours
3. customat room temperature
4. filtrationThen, the precipitate was collected by filtration
5. washwashed twice with 160 ml of warm 20% hydrous pyridine
6. customThe above-obtained reaction filtrate
7. washthe warm hydrous pyridine wash liquid
8. additionthe resulting solution was added to 1 liter of acetone
9. stirringby stirring for 24 hours
10. temperatureunder cooling with ice
11. filtrationThe precipitate was collected by filtration
12. additionwas added 70 ml of warm DMF
13. dissolutionto dissolve the precipitate
14. additionThen, 0.5 g of active carbon was added
15. stirringby stirring for 30 minutes at room temperature
16. filtrationInsoluble matter was filtered
17. addition8.4 ml of concentrated hydrochloric acid was added to the filtrate
18. additionThe resulting solution was added dropwise to 600 ml of acetone
19. stirringby stirring for 24 hours
20. temperatureunder cooling with ice
21. filtrationThen, the precipitate was collected by filtration