Iodine → 2-Chloro-3-iodopyridin-4-amine
反応式
[Cl:1][C:2]1[CH:7]=[C:6]([NH2:8])[CH:5]=[CH:4][N:3]=1.C(=O)([O-])[O-].[Na+].[Na+].[I-:15].[K+].II.[OH-].[Na+].S([O-])([O-])(=O)=S.[Na+].[Na+]>O>[Cl:1][C:2]1[C:7]([I:15])=[C:6]([NH2:8])[CH:5]=[CH:4][N:3]=1参加物
8
反応条件
- 温度
- 100 °C
実験手順
Commercially available 2-chloro-4-aminopyridine (15 g, 0.1 mol) and 37.2 g (0.4 mol) of sodium carbonate are suspended in 200 ml of water and warmed to 100° C. 58.3 g (0.4 mol) of potassium iodide and 59.4 g (0.2 mol) of iodine are added to the resultant solution, and the mixture is stirred at the temperature indicated for 12 h. The mixture is subsequently adjusted to pH 13 using sodium hydroxide solution, treated with sodium thiosulfate until completely decolorised and extracted with ethyl acetate. Chromatographic purification gives 5 g (17%) of solid.
後処理
- extractionextracted with ethyl acetate
- customChromatographic purification
出典と根拠
- ORDレコード
- ord-a5e1bc3944384b66943ecd4470c3c552
- 出典データセット
- uspto-grants-2014_10
- 特許番号
- US08859581B2
反応ノート
読み込み中…
