反应详情

温度

0 °C

H-Glu(OBzl)OBzl (2.0 g) was dissolved in a mixture of acetonitrile (50 ml) and water (10 ml). The solution was cooled to 0° C. and triethylamine (400 mg) and Boc-Lys(Z)OSu (1.91 g) were added. The mixture was stirred at 0°-5° C. for 2 hours and at room temperature for 3 hours. The solvent was distilled off and the residue was poured into a mixture of ethyl acetate (100 ml) and 2.5% hydrochloric acid. The organic layer was washed with water (50 ml×2), 2.5% sodium hydrogen carbonate (50 ml) and water (50 ml×3) in that order and dried over magnesium sulfate. The solvent was then distilled off to give Boc-Lys(Z)-Glu(OBzl)OBzl (2.70 g).

1. distillationThe solvent was distilled off
2. additionthe residue was poured into a mixture of ethyl acetate (100 ml) and 2.5% hydrochloric acid
3. washThe organic layer was washed with water (50 ml×2), 2.5% sodium hydrogen carbonate (50 ml) and water (50 ml×3) in that order
4. dry with materialdried over magnesium sulfate
5. distillationThe solvent was then distilled off