反应详情

温度

0 °C

H-Val-Gly-OBzl.HCl and Z-Glu-OBzl (5.57 g, 15.0 mmol) described above was dissolved in methylene chloride (50 ml), and the solution was maintained at 0° C. Triethylamine (2.30 ml, 16.5 mmol), HOBt (1-hydroxybenzotriazole, 2.53 g, 16.5 mmol) and WSC.HCl (1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride, 3.16 g, 16.5 mmol) were added to the solution, and the mixture was stirred at room temperature overnight for 2 days. The reaction solution was concentrated under reduced pressure, and the residue was dissolved in heated ethyl acetate (1,500 ml). The solution was washed with water (200 ml), 5% of citric acid aqueous solution (200 ml×twice), saturated brine (150 ml), 5% sodium hydrogen carbonate aqueous solution (200 ml×twice) and saturated brine (150 ml) again. The organic layer was dried over anhydrous magnesium sulfate, magnesium sulfate was removed by filtration, and the filtrate was concentrated under reduced pressure. The precipitated crystal was collected by filtration and dried under reduced pressure to obtain Z-Glu(Val-Gly-OBzl)-OBzl (6.51 g, 10.5 mmol) as a white crystal.

1. concentrationThe reaction solution was concentrated under reduced pressure
2. dissolutionthe residue was dissolved in heated ethyl acetate (1,500 ml)
3. washThe solution was washed with water (200 ml), 5% of citric acid aqueous solution (200 ml×twice), saturated brine (150 ml), 5% sodium hydrogen carbonate aqueous solution (200 ml×twice) and saturated brine (150 ml) again
4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate, magnesium sulfate
5. customwas removed by filtration
6. concentrationthe filtrate was concentrated under reduced pressure
7. filtrationThe precipitated crystal was collected by filtration
8. customdried under reduced pressure