Ethyl Acetate → 6-Phenoxy-3-pyridinamine
反応式
[N+:1]([C:4]1[CH:5]=[N:6][C:7]([O:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:8][CH:9]=1)([O-])=O.C(OCC)(=O)C>[Pd].C(O)C>[NH2:1][C:4]1[CH:5]=[N:6][C:7]([O:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:8][CH:9]=1参加物
5
実験手順
3-Nitro-6-phenoxypyridine (8.77 g, 40.6 mmol), 10% palladium on carbon (1.20 g) and 1:1 mixed solvent (250 mL) of ethyl acetate with ethanol were mixed and hydrogenation was performed at room temperature under an initial pressure of 196 kPa. After the catalyst was removed by filtration and washed with ethanol, the filtrate was concentrated. The residue was purified by silica gel chromatography (eluate n-hexane:ethyl acetate=1:1 v/v) to obtain 6.50 g (86%) of the title compound as faintly yellow needle-like crystals.
後処理
- customwas performed at room temperature
- customAfter the catalyst was removed by filtration
- washwashed with ethanol
- concentrationthe filtrate was concentrated
- customThe residue was purified by silica gel chromatography (eluate n-hexane:ethyl acetate=1:1 v/v)
出典と根拠
- ORDレコード
- ord-9f20b8e9516548a1b233845367cdbb6f
- 出典データセット
- uspto-grants-2007_02
- 特許番号
- US07176204B2
反応ノート
読み込み中…