反应详情

100 Milliliters of 20% hydrous pyridine was added to 3.0 g of 4-guanidinobenzoic acid.methanesulfonate, 3.0 g of 6-amidino-1-carbamoylmethyl-2-naphthol.hydrochloride and 4.5 g of DCC, followed by stirring for 2 hours under cooling with ice and then 2 days at room temperature. The precipitate was filtered and 1 g of active carbon was added to the filtrate, followed by stirring for 30 minutes under cooling with ice, and insoluble matter was filtered off. The filtrate was slowly added dropwise to 4 liters of ether under cooling with ice, followed by stirring for 2 hours. The precipitate was collected by filtration and washed with 100 ml of acetone to obtain a crude product. Then, the product was dissolved in 150 ml of methanol. Thereafter, 2.5 g of active carbon was added to the solution, followed by stirring for 30 minutes under cooling with ice, and insoluble matter was filtered off. The filtrate was slowly added dropwise to 1 liter of acetone under cooling with ice, followed by stirring for 2 hours. The precipitate was collected by filtration to obtain 2.9 g of the desired product.

1. temperatureunder cooling with ice
2. custom2 days
3. customat room temperature
4. filtrationThe precipitate was filtered
5. addition1 g of active carbon was added to the filtrate
6. stirringby stirring for 30 minutes
7. temperatureunder cooling with ice, and insoluble matter
8. filtrationwas filtered off
9. additionThe filtrate was slowly added dropwise to 4 liters of ether
10. temperatureunder cooling with ice
11. stirringby stirring for 2 hours
12. filtrationThe precipitate was collected by filtration
13. washwashed with 100 ml of acetone
14. customto obtain a crude product
15. additionThereafter, 2.5 g of active carbon was added to the solution
16. stirringby stirring for 30 minutes
17. temperatureunder cooling with ice, and insoluble matter
18. filtrationwas filtered off
19. additionThe filtrate was slowly added dropwise to 1 liter of acetone
20. temperatureunder cooling with ice
21. stirringby stirring for 2 hours
22. filtrationThe precipitate was collected by filtration