반응 #46063

반응 방정식

2-acetylpyridine

dichloromethane

2,3,5,6-tetramethyl-benzene-1,4-diamine

2-pyridinecarboxaldehyde

→

2,2′-bipyridinyl-6-carbaldehyde

6-acetyl-2,2′-bipyridine

용매

methanol

반응 조건

후처리

1. 1
   workup.ALIQUOTsampling accessories on a Perkin Elmer Spectrum One FTIR instrument
2. 2
   기타at ambient temperature
3. 3
   기타and used without further purification
4. 4
   기타used without further purification
5. 5
   기타All other chemicals were obtained commercially
6. 6
   기타used without further purification

실험 절차

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.

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