반응 #6711

ord-71d5c1e5a135455fba4054b6175a1d2a

용매

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the DMF was evaporated under reduced pressure
  2. 2
    workup.ADDITIONThe residue was diluted with ethyl acetate
  3. 3
    세척thoroughly washed with dilute aqueous HCl (pH 2), water, dilute aqueous NaOH (pH 9–10), and water
  4. 4
    건조The organic phase was dried over sodium sulfate
  5. 5
    기타evaporated to dryness
  6. 6
    기타to yield 9.2 g of the

실험 절차

3.74 g Z-D-Pro-OH (15 mmol, BACHEM) and 8.25 g H-Val-MeVal-Pro-Pro-NHBn×HCl (15 mmol) were dissolved in 80 ml dry DMF. After cooling to 0° C., 2.4 g DEPCN (2.25 ml, 15 mmol) and 4.2 ml triethylamine (30 mmol) were added. The reaction mixture was stirred at 0° C. for several hours and room temperature overnight, then the DMF was evaporated under reduced pressure. The residue was diluted with ethyl acetate and thoroughly washed with dilute aqueous HCl (pH 2), water, dilute aqueous NaOH (pH 9–10), and water. The organic phase was dried over sodium sulfate and evaporated to dryness to yield 9.2 g of the desired protected pentapeptide.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07084110B2uspto-grants-2006_08