Reaktion #1345546

Reaktionsgleichung

Z-(L)Glu(OtBu)-OH

EDCI hydrochloride

HOBT hydrate

DIPEA

DCM THF

→

desired compound

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

Lösungsmittel

water

DCM

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGThe mixture was stirred at RT overnight
2. 2
   Sonstigethe phases were separated
3. 3
   Waschenphase was washed with 2M Na2CO3, with 1M NaHSO4 and with brine
4. 4
   Trocknenwas dried (Na2SO4)
5. 5
   Sonstigeevaporated off
6. 6
   SonstigeDrying under HV

Vorschrift

To a solution of Z-(L)Glu(OtBu)-OH (25.2 g) in DCM/THF (240 mL/60 mL) were added EDCI hydrochloride (17.2 g), HOBT hydrate (13.7 g) and DIPEA (28.2 mL). After stirring at RT for 5 min, intermediate 1.2 (20 g) was added. The mixture was stirred at RT overnight. DCM and water were added and the phases were separated. The org. phase was washed with 2M Na2CO3, with 1M NaHSO4 and with brine, was dried (Na2SO4) and evaporated off. Drying under HV gave the desired compound as an orange oil (40 g).

Quelle