4-Chloro-2-iodophenol → 5-Chloro-2-hydroxybenzonitrile
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4](I)[CH:3]=1.[Cu](C#N)[C:11]#[N:12]>CN(C=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([CH:3]=1)[C:11]#[N:12]参加物
4
実験手順
4-Chloro-2-iodophenol (85 g, 0.33 mol) was dissolved in 150 ml of DMF, followed by the addition of 32.5 g (0.36 mol) of copper cyanide. The resulting mixture was refluxed for 2 hours and then concentrated under reduced pressure. The residue was dissolved in ethyl acetate, and the thus-prepared solution was washed with water. Subsequent to elimination of an undissolved salt, the solution was concentrated under reduced pressure, whereby 40.4 g of 5-chloro-2-hydroxybenzonitrile were obtained (yield: 80%). Without purification, it was provided for use in the next step.
後処理
- temperatureThe resulting mixture was refluxed for 2 hours
- concentrationconcentrated under reduced pressure
- dissolutionThe residue was dissolved in ethyl acetate
- washthe thus-prepared solution was washed with water
- concentrationSubsequent to elimination of an undissolved salt, the solution was concentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-f3352d88e25148b4acc039e8361129c1
- 出典データセット
- uspto-grants-2000_10
- 特許番号
- US06136848
反応ノート
読み込み中…