反应详情

50 Milliliters of anhydrous pyridine was added to 1.9 g of 4-aminoiminomethylaminobenzoic acid.hydro-chloride, 3.0 g of of 6-amidino-1-methoxycarbonyl-2-naphthol.methanesulfonate, and 2.2 g of DCC, followed by stirring for 2 hours under cooling with ice and 24 hours at room temperature. The precipitate was collected by filtration and washed with a small amount of pyridine. To the collected precipitate was added 30 ml of water, followed by stirring for 1 hour. Insoluble matter was filtered off and the filtrate was added dropwise to 100 ml of saturated aqueous sodium bicarbonate solution, followed by stirring for 24 hours under cooling with ice. Then, the precipitate was collected by filtration and washed with a small amount of water and acetone. To the collected precipitate were added 15 ml of methanol and 2.2 ml of methanesulfonic acid. The resulting solution was added dropwise to 300 ml of ether, followed by stirring for 24 hours under cooling with ice. Then, the precipitate was collected by filtration and washed with a small amount of acetone to obtain 2.46 g of the desired product.

1. filtrationThe precipitate was collected by filtration
2. washwashed with a small amount of pyridine
3. additionTo the collected precipitate was added 30 ml of water
4. stirringby stirring for 1 hour
5. filtrationInsoluble matter was filtered off
6. additionthe filtrate was added dropwise to 100 ml of saturated aqueous sodium bicarbonate solution
7. stirringby stirring for 24 hours
8. temperatureunder cooling with ice
9. filtrationThen, the precipitate was collected by filtration
10. washwashed with a small amount of water and acetone
11. additionTo the collected precipitate were added 15 ml of methanol and 2.2 ml of methanesulfonic acid
12. additionThe resulting solution was added dropwise to 300 ml of ether
13. stirringby stirring for 24 hours
14. temperatureunder cooling with ice
15. filtrationThen, the precipitate was collected by filtration
16. washwashed with a small amount of acetone