Reaktion #46063

ord-cd4a0fbf8960475d98c2646ed156d769

Reaktionsgleichung

CC(=O)c1ccccn1
2-acetylpyridine
ClCCl
dichloromethane
Cc1c(C)c(N)c(C)c(C)c1N
2,3,5,6-tetramethyl-benzene-1,4-diamine
O=Cc1ccccn1
2-pyridinecarboxaldehyde
O=Cc1cccc(-c2ccccn2)n1
2,2′-bipyridinyl-6-carbaldehyde
CC(=O)c1cccc(-c2ccccn2)n1
6-acetyl-2,2′-bipyridine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ALIQUOTsampling accessories on a Perkin Elmer Spectrum One FTIR instrument
  2. 2
    Sonstigeat ambient temperature
  3. 3
    Sonstigeand used without further purification
  4. 4
    Sonstigeused without further purification
  5. 5
    SonstigeAll other chemicals were obtained commercially
  6. 6
    Sonstigeused without further purification

Vorschrift

The electrospray (ES) mass spectra were recorded using a micromass Quattra LC mass spectrometer with dichloromethane or methanol as the matrix [Masslynx software. open-access autosampler injection]. The infrared spectra were recorded with Universal ATR sampling accessories on a Perkin Elmer Spectrum One FTIR instrument. 1H and 13C NMR spectra were recorded on a Bruker ARX spectrometer 250/300 MHz at ambient temperature; chemical shifts (ppm) are referred to the residual protic solvent peaks. The reagents 2-pyridinecarboxaldehyde, the 2-acetylpyridine, 2,3,5,6-tetramethyl-benzene-1,4-diamine were purchased from Aldrich Chemical Co. and used without further purification. Formic acid (98%) was purchased from Fisons PLC and used without further purification. The compounds 2,2′-bipyridinyl-6-carbaldehyde [J. Uenishi, T. Tanaka, K. Nishiwaki, S. Wakabayashi, S. Oae and H. Tsukube, J. Org. Chem., 1993, 58, 4382], 6-acetyl-2,2′-bipyridine [J. Uenishi, T. Hiraoka, S. Hata, K. Nishiwaki and O. Yonemitsu, J. Org. Chem., 1998, 63, 2481] were prepared according to the indicated journal articles. All other chemicals were obtained commercially and used without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07741240B2uspto-grants-2010_06