Reaktion #1269839

ord-91cccc8fe93f40d99bcf8c3ba833bdba

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 is concentrated under vacuum, water
  2. 2
    workup.ADDITIONis added to the residue
  3. 3
    Extraktionthe product is extracted with ethyl acetate
  4. 4
    SonstigeThe crude product is purified by conversion into its hydrochloride salt

Vorschrift

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

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08664193B2uspto-grants-2014_03