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

HRID 17785

반응식

HRID 17785 반응식
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]

참가 물질

7

반응물 4

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

생성물 2

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

시약·촉매·용매 1

HCID 887Methanol용매

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cd4a0fbf8960475d98c2646ed156d769
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07741240B2

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