Reaktion #434780

Reaktionsgleichung

H-Glu(O-t-Bu)-OH

EDC

HOBt

→

2-amino-pentanedioic acid 5-tert-butyl ester 1-ethyl ester

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe solvent was removed under reduced pressure
2. 2
   workup.DISSOLUTIONthe resulting oil was dissolved in dichloromethane 300 mL
3. 3
   Extraktionextracted with H2O 300 mL
4. 4
   ExtraktionThe crude product was extracted into dichloromethane 400 mL
5. 5
   Trocknendried over NaSO4
6. 6
   Filtrationfiltrated
7. 7
   Sonstigeevaporated

Vorschrift

A dry 250 mL round-bottomed flask was charged with 2.200 g (10.800 mmol) H-Glu(O-t-Bu)-OH (41a) dissolved in 100 mL ethanol. To this was added 4.4 g (22.9 mmol) EDC and 3.2 g (23.7 mmol) HOBt. The reaction mixture was stirred at ambient temperature for 22 h. The reaction mixture was followed to completion according to the LC-MS data. The solvent was removed under reduced pressure and the resulting oil was dissolved in dichloromethane 300 mL and extracted with H2O 300 mL. The H2O-phase was adjusted to pH 9.5. The crude product was extracted into dichloromethane 400 mL, dried over NaSO4, filtrated and evaporated.

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