反应 #969878

反应方程式

triethylamine

BOP

Z-Val-Pro-OH

H-Val-Pro-OtBu.HCl

→

Z-Val-Pro-Val-Pro-OtBu

收率 68.0%

溶剂

dichloromethane

反应条件

后处理

1. 1
   其他Then, the solvent was evaporated
2. 2
   workup.DISSOLUTIONthe residue was dissolved in dichloromethane
3. 3
   洗涤washed with citric acid (10%), NaHCO3 (10%) and brine
4. 4
   干燥The organic layer was dried (Na2SO4)
5. 5
   其他evaporated to dryness
6. 6
   其他leaving a residue that
7. 7
   其他was purified on a column chromatography with hexane-ethyl acetate, 2:1
8. 8
   其他to give X (68% yield)

实验过程

A solution of Z-Val-Pro-OH (681.3 mg, 1.95 mmol) in dichloromethane (6 mL), was successively treated at room temperature. with (benzotriazol-1-yloxy)tris(dimethylamino)phosphoniun hexafluorophale (BOP) (865.1 mg, 1.95 mmol), H-Val-Pro-OtBu.HCl (500 mg, 1.63 mmol) and triethylamine (TEA) (500 μL, 3.58 mmol). The mixture was stirred overnight at room temperature. Then, the solvent was evaporated, the residue was dissolved in dichloromethane and washed with citric acid (10%), NaHCO3 (10%) and brine. The organic layer was dried (Na2SO4) and evaporated to dryness leaving a residue that was purified on a column chromatography with hexane-ethyl acetate, 2:1 to give X (68% yield).

来源