Reaktion #75559

Reaktionsgleichung

H-Pro-OBzl

Boc-Val-OH

HOBt

NMM

DCC

→

Boc-Val-Pro-OBzl

Lösungsmittel

chloroform

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe mixture was filtered
2. 2
   Sonstigesolvent was evaporated
3. 3
   workup.ADDITIONEthyl acetate was added
4. 4
   Sonstigeinsoluble material was removed by filtration
5. 5
   WaschenThe filtrate was washed with 0.2N HCl, 5% NaHCO3, and saturated aqueous NaCl
6. 6
   TrocknenIt was dried over Na2SO4
7. 7
   Filtrationfiltered
8. 8
   Sonstigeevaporate

Vorschrift

Boc-Val-Pro-OBzl was prepared by dissolving H-Pro-OBzl (20 g, 83 mmol) in 50 mL of chloroform and adding Boc-Val-OH (18.0 g, 83 mmol), HOBt (23.0g, 165 mmol), NMM ( 9.0 mL, 83 mmol) and DCC (17.0 g, 83 mmol). The reaction mixture was stirred overnight at room temperature. The mixture was filtered and solvent was evaporated. Ethyl acetate was added and insoluble material was removed by filtration. The filtrate was washed with 0.2N HCl, 5% NaHCO3, and saturated aqueous NaCl. It was dried over Na2SO4, filtered and evaporate to give a white solid (30 g, 75 mmol, 90%). ESI/MS calculated for C22H32N2O5 +H: 405.2. Found 405.6.

Quelle