تفاعل #969873

معادلة التفاعل

Z-Val-Pro-Val-Pro-OH

1-hydroxibenzotriazol

N,N′-diisopropylcarbodiimide

Ara-C

→

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

المردود 22.0%

المذيبات

dimethylformamide

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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)

المصدر