反应详情

Into 50 ml of anhydrous pyridine, was dissolved 3.3 g of 3-benzyloxycarbonylaminopropionic acid. To the solution, while being cooled in ice, was added 3.7 g of DCC. The mixture was stirred for 30 minutes. After addition of 5.0 g of 4-amidino-2-benzoylphenol methanesulfonate, the mixture was further stirred overnight. The precipitate which was formed was separated by filtration and washed with pyridine. Ethyl ether was added to the filtrate to separate an oily substance which solidified upon stirring. The solidified substance was collected by filtration, washed with ethyl ether, and dissolved in DMF. The crystals precipitated out of the DMF solution by the addition of ethyl ether were recrystallized from ethanol to yield 3.9 g of colorless granular crystals of 4-amidino-2-benzoylphenyl 3-benzyloxycarbonylaminopropionate methanesulfonate.

1. temperatureTo the solution, while being cooled in ice
2. waitthe mixture was further stirred overnight
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 separate an oily substance which
8. stirringupon stirring
9. filtrationThe solidified substance was collected by filtration
10. washwashed with ethyl ether
11. dissolutiondissolved in DMF
12. customThe crystals precipitated out of the DMF solution by the addition of ethyl ether
13. customwere recrystallized from ethanol