Reaktion #60126

ord-25669a844f034f04b49514e88526da2a

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    EinengenThe reaction mixture was concentrated in vacuo
  2. 2
    workup.ADDITIONdiluted with water and ethyl acetate
  3. 3
    ExtraktionThe solution was extracted three times with ethyl acetate
  4. 4
    Trocknendried over sodium sulfate
  5. 5
    Sonstigepurified by column chromatography
  6. 6
    Wascheneluting with 5-10% methanol/methylene chloride

Vorschrift

1 mmol of 2-(2,4-dichlorophenyl)-6-chloro-3-nitropyridine was taken with 2 mmol of (2-aminoethyl)(6-amino-5-nitro(2-pyridyl))amine and 3 mmol of N,N-diisopropylethylamine in 2 ml of DMF at 80° C. for two hours. The reaction mixture was concentrated in vacuo and diluted with water and ethyl acetate. The solution was extracted three times with ethyl acetate, dried over sodium sulfate, and purified by column chromatography eluting with 5-10% methanol/methylene chloride to obtain {2-[(6-amino-5-nitro(2-pyridyl))amino]ethyl}[6-(2,4-dichlorophenyl)-5-nitro(2-pyridyl)]amine.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07425557B2uspto-grants-2008_09