反応 #969878

反応方程式

triethylamine

BOP

Z-Val-Pro-OH

H-Val-Pro-OtBu.HCl

→

Z-Val-Pro-Val-Pro-OtBu

収率 68.0%

溶媒

dichloromethane

反応条件

後処理

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

実験手順

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).

出典