2-(3-Nitrophenyl)pyridine → 3-(2-Pyridyl)aniline
反応式
[N+:1]([C:4]1[CH:5]=[C:6]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][N:11]=2)[CH:7]=[CH:8][CH:9]=1)([O-])=O.[H][H]>[Pd].C(O)C>[N:11]1[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=1[C:6]1[CH:5]=[C:4]([CH:9]=[CH:8][CH:7]=1)[NH2:1]参加物
5
実験手順
To a solution of 2-(3-nitrophenyl)pyridine (prepared as described in J. Chem. Soc. 1958 p. 1759) (12.7 g, 63.5 mmol) in abs. ethanol is added palladium catalyst (1.3 g 5% Pd on activated carbon) and the mixture is hydrogenated at ambient pressure until the hydrogen uptake has ceased. The mixture is filtered through celite and the filtrate is concentrated under reduced pressure. The residue is purified by column-chromatography on silica gel using a mixture of ethyl acetate and petroleum ether (9:1) as the eluent to afford 2f (9.5 g, 88%) as a light brown oil.
後処理
- filtrationThe mixture is filtered through celite
- concentrationthe filtrate is concentrated under reduced pressure
- customThe residue is purified by column-chromatography on silica gel using
- additiona mixture of ethyl acetate and petroleum ether (9:1) as the eluent
出典と根拠
- ORDレコード
- ord-c560b47ac9cf41dea241c965f4ff3c10
- 出典データセット
- uspto-grants-1999_07
- 特許番号
- US05922724
反応ノート
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