反应详情

Into 50 ml of anhydrous pyridine, was dissolved 4.0 g of 6-benzyloxycarbonylaminocaproic acid. To the solution, while being cooled in ice, was added 3.7 g of DCC. After having been stirred for 30 minutes, the mixture was admixed with 5.0 g of 4-amidino-2-benzoylphenol methanesulfonate and stirred overnight at room temperature. The precipitate which was formed was separated by filtration and washed with pyridine. Ethyl ether was added to the filtrate to precipitate white crystals. The crystals were collected by filtration, washed with ethyl ether, dissolved in DMF, and admixed with ethyl ether to precipitate colorless crystals which were collected by filtration and dried to obtain 5.7 g of an anhydrous substance. This substance was recrystallized from ethanol to obtain 2.7 g of colorless needle crystals of 4-amidino 2-benzoylphenyl 6-benzyloxycarbonylaminocaproate methanesulfonate.

1. temperatureTo the solution, while being cooled in ice
2. stirringstirred overnight at room temperature
3. customThe precipitate which was formed
4. customwas separated by filtration
5. washwashed with pyridine
6. additionEthyl ether was added to the filtrate
7. customto precipitate white crystals
8. filtrationThe crystals were collected by filtration
9. washwashed with ethyl ether
10. dissolutiondissolved in DMF
11. customto precipitate colorless crystals which
12. filtrationwere collected by filtration
13. customdried
14. customto obtain 5.7 g of an anhydrous substance
15. customThis substance was recrystallized from ethanol