Reaktion #640991

Reaktionsgleichung

1-ethoxycarbonylpiperazine

NaHCO3

Z-(L)Glu(OtBu)—OH

HOBT hydrate

EDCI hydrochloride

→

desired compound

Ausbeute 98.9%

4-((S)-2-benzyloxycarbonylamino-4-tert-butoxycarbonyl-butyryl)-piperazine-1-carboxylic acid ethyl ester

Ausbeute 98.9%

Lösungsmittel

EA

DCM THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.WAITthe stirring was continued overnight at RT
2. 2
   Sonstigethe phases were separated
3. 3
   Waschenphase was washed with 60 ml of a 1M NaHSO4 solution and 60 ml of a NaCl solution
4. 4
   Trocknenwas dried (Na2SO4)
5. 5
   Sonstigeevaporated off
6. 6
   SonstigeAfter HV drying

Vorschrift

Z-(L)Glu(OtBu)—OH (5 g), HOBT hydrate (2.5 g) and EDCI hydrochloride (3.1 g) were dissolved in DCM/THF (1/1, 42 ml). After 15 min stirring, 1-ethoxycarbonylpiperazine (2.6 g) was added and the stirring was continued overnight at RT. 150 ml of EA and 60 ml of a NaHCO3 solution were added to the mixture and the phases were separated. The org. phase was washed with 60 ml of a 1M NaHSO4 solution and 60 ml of a NaCl solution, was dried (Na2SO4) and evaporated off. After HV drying, 7 g of the desired compound were obtained.

Quelle