Hydrochloric Acid → 5-Bromo-2-iodopyridin-3-ol
反応式
[Br:1][C:2]1[CH:3]=[C:4]([OH:8])[CH:5]=[N:6][CH:7]=1.C(=O)([O-])[O-].[Na+].[Na+].[I:15]I.Cl>O>[Br:1][C:2]1[CH:3]=[C:4]([OH:8])[C:5]([I:15])=[N:6][CH:7]=1参加物
6
実験手順
To a solution of 5-bromopyridin-3-ol (2.75 g, 15.8 mmol) and sodium carbonate (3.35 g, 31.6 mmol) in water (45 mL) was added iodine (4.01 g, 15.8 mmol), and the mixture was stirred at room temperature for 1 hr. 6N Hydrochloric acid (7 mL) was added thereto, and the mixture was weakly acidified with 1N hydrochloric acid (about 5 mL) (pH 4). The resulting solid was collected, washed with water and dissolved in ethyl acetate. The solution was washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the obtained solid was washed with a small amount of acetonitrile to give the title compound (3.57 g, yield 75%).
後処理
- customThe resulting solid was collected
- washwashed with water
- dissolutiondissolved in ethyl acetate
- washThe solution was washed with saturated brine
- dry with materialdried over anhydrous sodium sulfate
- customThe solvent was evaporated under reduced pressure
- washthe obtained solid was washed with a small amount of acetonitrile
出典と根拠
- ORDレコード
- ord-c0c7771bd99a497b94dc512b24f98020
- 出典データセット
- uspto-grants-2013_08
- 特許番号
- US08501804B2
反応ノート
読み込み中…