反应详情

To 4.6 g of 4-t-butoxycarbonyl-2-guanidinobutyric acid hydrochloride, 5.3 g of 6-amidino-2-naphthyl 5-aminomethylfuran-2-carboxylate dihydrobromide and 220 mg of DMAP were added 110 ml of DMA and 36 ml of pyridine and the resulting mixture was stirred while cooling with ice. After 10 minutes, 4 g of DCC was added and the mixture was stirred for 3 hours while cooling with ice and then for 16 hours at room temperature. The precipitated were filtered off, the filtrate was added in small portions into 3 l of ether and stirred at room temperature for 3 hours. After removing the supernatant by decantation, the residue was dissolved in 60 ml of DMF, then 3 g of active carbon was added thereto, and the mixture was stirred for 30 minutes while cooling with ice. The insolubles were filtered off, and the filtrate was added dropwise into 3 l of ether and stirred for 5 hours while cooling with ice. The crystals thus precipitated were collected by filtration to obtain 6.7 g of the intended product.

1. temperaturewhile cooling with ice
2. stirringthe mixture was stirred for 3 hours
3. temperaturewhile cooling with ice
4. waitfor 16 hours at room temperature
5. filtrationThe precipitated were filtered off
6. additionthe filtrate was added in small portions into 3 l of ether
7. stirringstirred at room temperature for 3 hours
8. customAfter removing the supernatant by decantation
9. dissolutionthe residue was dissolved in 60 ml of DMF
10. addition3 g of active carbon was added
11. stirringthe mixture was stirred for 30 minutes
12. temperaturewhile cooling with ice
13. filtrationThe insolubles were filtered off
14. additionthe filtrate was added dropwise into 3 l of ether
15. stirringstirred for 5 hours
16. temperaturewhile cooling with ice
17. customThe crystals thus precipitated
18. filtrationwere collected by filtration