反应 #969873

反应方程式

Z-Val-Pro-Val-Pro-OH

1-hydroxibenzotriazol

N,N′-diisopropylcarbodiimide

Ara-C

→

Z-Val-Pro-Val-Pro Ara-C

收率 22.0%

溶剂

dimethylformamide

反应条件

后处理

1. 1
   其他was continued until complete disappearance of the starting material (overnight)
2. 2
   其他Then, the solvent was evaporated
3. 3
   workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
4. 4
   洗涤washed with citric acid (10%), NaHCO3 (10%) and brine
5. 5
   干燥The organic layer was dried (Na2SO4)
6. 6
   其他evaporated to dryness
7. 7
   其他leaving a residue that
8. 8
   其他was purified by CCTLC on the chromatotron with dichloromethane:methanol (20:1)
9. 9
   其他to give D (22% yield)

实验过程

A solution of Z-Val-Pro-Val-Pro-OH [SEQ ID NO:9] (134.4 mg, 0.24 mmol) in dimethylformamide (1.5 mL), was successively treated at room temperature with 1-hydroxibenzotriazol (33.3 mg, 0.24 mmol), N,N′-diisopropylcarbodiimide (38.4 μL, 0.24 mmol) and Ara-C (50 mg, 0.20 mmol). The stirring was continued until complete disappearance of the starting material (overnight). Then, the solvent was evaporated, and the residue was dissolved in ethyl acetate 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 by CCTLC on the chromatotron with dichloromethane:methanol (20:1) to give D (22% yield)

来源