反应 #6711
ord-71d5c1e5a135455fba4054b6175a1d2a
反应方程式
triethylamine
Z-D-Pro-OH
H-Val-MeVal-Pro-Pro-NHBn
HCl
→
Z-D-Pro-Val-MeVal-Pro-Pro-NHBn
溶剂
反应条件
温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他the DMF was evaporated under reduced pressure
- 2workup.ADDITIONThe residue was diluted with ethyl acetate
- 3洗涤thoroughly washed with dilute aqueous HCl (pH 2), water, dilute aqueous NaOH (pH 9–10), and water
- 4干燥The organic phase was dried over sodium sulfate
- 5其他evaporated to dryness
- 6其他to yield 9.2 g of the
实验过程
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.