4-Chloro-2-iodophenol → 5-Chloro-2-hydroxybenzonitrile
반응식
[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]참가 물질
4
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-f3352d88e25148b4acc039e8361129c1
- 출처 데이터셋
- uspto-grants-2000_10
- 특허 번호
- US06136848
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