Reaktion #343674

Reaktionsgleichung

H-Gly-OEt.HCl

Boc-Val-OH

HOBT

WSC.HCl

→

Boc-Val-Gly-OEt

Ausbeute 85.3%

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenThe reaction mixture was concentrated under reduced pressure
2. 2
   workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
3. 3
   Waschensuccessively washed three times with 1N hydrochloric acid
4. 4
   Trocknenonce with saturated aqueous sodium chloride, three times with 5% aqueous sodium hydrogen carbonate, three times with saturated aqueous sodium chloride, and dried over anhydrous sodium sulfate
5. 5
   Einengenfollowed by concentration under reduced pressure
6. 6
   SonstigeThe residue was recrystallized from ethyl acetate-n-hexane

Vorschrift

To a solution of 3.21 g of the H-Gly-OEt.HCl dissolved in 10 ml of DMF, under cooling at -5° C., 5.00 g of Boc-Val-OH, 3.10 g of HOBT and 4.79 g of WSC.HCl were added, and the mixture was stirred at -5° C. for one hour and at room temperature overnight. The reaction mixture was concentrated under reduced pressure, and the residue was dissolved in ethyl acetate, successively washed three times with 1N hydrochloric acid, once with saturated aqueous sodium chloride, three times with 5% aqueous sodium hydrogen carbonate, three times with saturated aqueous sodium chloride, and dried over anhydrous sodium sulfate, followed by concentration under reduced pressure. The residue was recrystallized from ethyl acetate-n-hexane to give 5.93 g (yield: 85.2%) of Boc-Val-Gly-OEt melting at 91.5° to 93° C.

Quelle