反应 #1365718

反应方程式

HCl

Z-Leu-OSu

H-Asp(OtBu)-Leu-OH

sodium bicarbonate

→

Z-Leu-Asp(OtBu)-Leu-OH

收率 80.7%

溶剂

dioxane

water

反应条件

后处理

1. 1
   其他to give
2. 2
   workup.ADDITIONa mixture of pH 8
3. 3
   萃取was extracted with ethyl acetate (30 mL×3)
4. 4
   干燥The combined extracts were dried over Na2SO4
5. 5
   过滤filtered
6. 6
   浓缩concentrated
7. 7
   workup.DISSOLUTIONThe crude product was dissolved in methanol
8. 8
   其他chromatographed on a column of Sephadex™ LH20

实验过程

The H-Asp(OtBu)-Leu-OH (3.02 g), sodium bicarbonate (1.68 g), and 30 mL of water were mixed to give a mixture of pH 8. Z-Leu-OSu (3.63 g) in dioxane (30 mL) was added to the mixture and was stirred at room temp for 2 h. The reaction mixture was acidified by addition of conc. HCl to pH 1.0, then was extracted with ethyl acetate (30 mL×3). The combined extracts were dried over Na2SO4, filtered, and concentrated. The crude product was dissolved in methanol and chromatographed on a column of Sephadex™ LH20 to yield Z-Leu-Asp(OtBu)-Leu-OH as a foamy solid (4.43 g).

来源