Reaktion #660089

ord-602c9adf23a2467b91482d774345083c

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 can be concentrated under vacuum, water
  2. 2
    workup.ADDITIONcan be added to the residue
  3. 3
    Extraktionthe product can be extracted with ethyl acetate
  4. 4
    SonstigeThe crude product can be 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) can be dissolved in 20% piperidine in dimethylformamide at 0° C. The solution can be stirred continuously for 1 h. The reaction mixture can be concentrated under vacuum, water can be added to the residue, and the product can be extracted with ethyl acetate. The crude product can be purified by conversion into its hydrochloride salt.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09029525B2uspto-grants-2015_05