Dichloromethane → (2,2'-Bipyridine)-6-carbaldehyde

HRID 17785

反応式

HRID 17785 の反応式
ClCCl.[N:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[CH:10]=[O:11].[C:12]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][N:16]=1)(=[O:14])[CH3:13].CC1[C:27](C)=[C:26](N)[C:25](C)=[C:24](C)[C:23]=1[NH2:32]>CO>[N:4]1[C:5]([CH:10]=[O:11])=[CH:6][CH:7]=[CH:8][C:9]=1[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][N:16]=1.[C:12]([C:15]1[N:16]=[C:17]([C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][N:32]=2)[CH:18]=[CH:19][CH:20]=1)(=[O:14])[CH3:13]

参加物

7

反応物 4

HCID 6344DichloromethaneHCID 142732-PyridinecarboxaldehydeHCID 142862-AcetylpyridineHCID 765482,3,5,6-Tetramethyl-1,4-phenylenediamine

生成物 2

HCID 11095276(2,2'-Bipyridine)-6-carbaldehydeHCID 158275201-([2,2'-Bipyridin]-6-yl)ethanone

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  1. aliquotsampling accessories on a Perkin Elmer Spectrum One FTIR instrument
  2. customat ambient temperature
  3. customand used without further purification
  4. customused without further purification
  5. customAll other chemicals were obtained commercially
  6. customused without further purification

出典と根拠

ORDレコード
ord-cd4a0fbf8960475d98c2646ed156d769
出典データセット
uspto-grants-2010_06
特許番号
US07741240B2

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