Reaktion #49168

ord-ff07496bf4054a7eaff388a58049f106

Reaktionsgleichung

CCOC(=O)CCN(CC(=O)OCC)C(=O)CCCCCNC(=O)OCC1c2ccccc2-c2ccccc21
3-{Ethoxycarbonylmethyl-[6-(9H-fluoren-9-ylmethoxycarbonylamino)-hexanoyl]-amino}-propionic acid ethyl ester
CCOC(=O)CCN(CC(=O)OCC)C(=O)CCCCCN
3-[(6-Amino-hexanoyl)-ethoxycarbonylmethyl-amino]-propionic acid ethyl ester

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe reaction mixture was concentrated in vacuum
  2. 2
    workup.ADDITIONthe residue water was added
  3. 3
    Extraktionthe product was extracted with ethyl acetate
  4. 4
    SonstigeThe crude product was purified

Vorschrift

3-{Ethoxycarbonylmethyl-[6-(9H-fluoren-9-ylmethoxycarbonylamino)-hexanoyl]-amino}-propionic acid ethyl ester AB (11.5 g, 21.3 mmol) was dissolved in 20% piperidine in dimethylformamide at 0° C. The solution was continued stirring for 1 h. The reaction mixture was concentrated in vacuum and the residue water was added and the product was extracted with ethyl acetate. The crude product was purified by converting into hydrochloride salt.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07745608B2uspto-grants-2010_06