2-Chloro-4-cyanopyridine → 2-Methoxyisonicotinonitrile

HRID 260471

反応式

HRID 260471 の反応式
Cl[C:2]1[CH:7]=[C:6]([C:8]#[N:9])[CH:5]=[CH:4][N:3]=1.[CH3:10][O-:11].[Na+]>CO>[C:8]([C:6]1[CH:5]=[CH:4][N:3]=[C:2]([O:11][CH3:10])[CH:7]=1)#[N:9]

参加物

4

実験手順

A solution of 2-chloro-4-cyanopyridine (1.25 g, 9.1 mmol), prepared as described by D. Libermann, N. Rist, F. Grumbach, S. Cals, M. Moyeux and A. Rouaix, Bull. Soc. Chim. France, 694 (1958), in methanol was treated with sodium methoxide (0.58 g, 10.9 mmol) and refluxed for 30 minutes. The reaction mixture was cooled, filtered and the filtrate concentrated in vacuo to obtain the crude product as an off-white solid. The crude product was chromatographed on silica gel with 20% ethyl acetate in hexane. The title compound was obtained as a white powder.

後処理

  1. temperaturerefluxed for 30 minutes
  2. temperatureThe reaction mixture was cooled
  3. filtrationfiltered
  4. concentrationthe filtrate concentrated in vacuo
  5. customto obtain the crude product as an off-white solid
  6. customThe crude product was chromatographed on silica gel with 20% ethyl acetate in hexane

出典と根拠

ORDレコード
ord-45dee7e4a0c54f2d8932178cdf3a380e
出典データセット
uspto-grants-1996_06
特許番号
US05527819

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