تفاعل #969878

معادلة التفاعل

triethylamine

BOP

Z-Val-Pro-OH

H-Val-Pro-OtBu.HCl

→

Z-Val-Pro-Val-Pro-OtBu

المردود 68.0%

المذيبات

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   أخرىThen, the solvent was evaporated
2. 2
   workup.DISSOLUTIONthe residue was dissolved in dichloromethane
3. 3
   غسيلwashed with citric acid (10%), NaHCO3 (10%) and brine
4. 4
   تجفيفThe organic layer was dried (Na2SO4)
5. 5
   أخرىevaporated to dryness
6. 6
   أخرىleaving a residue that
7. 7
   أخرىwas purified on a column chromatography with hexane-ethyl acetate, 2:1
8. 8
   أخرىto give X (68% yield)

الإجراء التجريبي

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).

المصدر