反应详情

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)

1. customwas continued until complete disappearance of the starting material (overnight)
2. customThen, the solvent was evaporated
3. dissolutionthe residue was dissolved in ethyl acetate
4. washwashed with citric acid (10%), NaHCO3 (10%) and brine
5. dry with materialThe organic layer was dried (Na2SO4)
6. customevaporated to dryness
7. customleaving a residue that
8. customwas purified by CCTLC on the chromatotron with dichloromethane:methanol (20:1)
9. customto give D (22% yield)