Hydrochloric Acid → 5-Fluoro-4-methylpyridin-2-amine
反応式
[F:1][C:2]1[C:3]([CH3:12])=[CH:4][C:5]([NH:8]C(=O)C)=[N:6][CH:7]=1.Cl>C(O)C>[F:1][C:2]1[C:3]([CH3:12])=[CH:4][C:5]([NH2:8])=[N:6][CH:7]=1参加物
4
実験手順
The N1-(5-fluoro-4-methyl-2-pyridyl)acetamide (4.25 g, 25.3 mmol) obtained in (D) was dissolved in ethanol (3ml), added with 6 M aqueous hydrochloric acid (3ml) and refluxed by heating for 1 hour and 30 minutes. The reaction mixture was left stand for cooling and the solvent was concentrated. The resulting residue was dissolved in distilled water, and the system was made basic with 1 N aqueous sodium hydroxide and extracted twice with chloroform. The organic layer was dried over anhydrous magnesium sulfate and the solvent was evaporated to obtain the title compound (2.82 g, 88%) as solid.
後処理
- temperaturerefluxed
- temperatureby heating for 1 hour and 30 minutes
- waitThe reaction mixture was left stand
- temperaturefor cooling
- concentrationthe solvent was concentrated
- dissolutionThe resulting residue was dissolved in distilled water
- extractionextracted twice with chloroform
- dry with materialThe organic layer was dried over anhydrous magnesium sulfate
- customthe solvent was evaporated
出典と根拠
- ORDレコード
- ord-c862f786502646c3836b4dfaa4c56ff7
- 出典データセット
- uspto-grants-2006_06
- 特許番号
- US07056917B2
反応ノート
読み込み中…