반응 #6711
ord-71d5c1e5a135455fba4054b6175a1d2a
용매
반응 조건
온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타the DMF was evaporated under reduced pressure
- 2workup.ADDITIONThe residue was diluted with ethyl acetate
- 3세척thoroughly washed with dilute aqueous HCl (pH 2), water, dilute aqueous NaOH (pH 9–10), and water
- 4건조The organic phase was dried over sodium sulfate
- 5기타evaporated to dryness
- 6기타to 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.