4-Chlorobenzonitrile → 4-Fluorobenzonitrile

HRID 9924

反応式

HRID 9924 の反応式
Cl[C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=1.[F-:10].[K+]>CS(C)=O>[F:10][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=1

参加物

4

反応条件

温度
180 °C

実験手順

200 g of 4-chlorobenzonitrile, 101.4 g of potassium fluoride, 25 g of dimethyl sulfoxide, and 5.60 g of (N,N-dimethylimidazolidino)tetramethyl-guanidinium chloride were placed in a 1 liter 4-neck flask equipped with anchor stirrer, thermometer, and reflux condenser with bubble counter. The mixture was then heated with stirring to 180° C. and this temperature was maintained for 16 hours. The mixture was then cooled to room temperature, water was added to the reaction mixture in a volumetric ratio of 1:1, and the mixture was extracted with diethyl ether. After washing, concentration, and drying the separated organic phase, 4-fluorobenzo-nitrile was isolated in a yield of 75%.

後処理

  1. customequipped with anchor stirrer
  2. temperaturethermometer, and reflux condenser
  3. customwith bubble counter
  4. temperatureThe mixture was then heated
  5. temperaturethis temperature was maintained for 16 hours
  6. temperatureThe mixture was then cooled to room temperature
  7. additionwater was added to the reaction mixture in a volumetric ratio of 1:1
  8. extractionthe mixture was extracted with diethyl ether
  9. washAfter washing
  10. concentrationconcentration
  11. customdrying the separated organic phase

出典と根拠

ORDレコード
ord-86800bf9397e44b882523bdaca98c2ce
出典データセット
uspto-grants-2006_08
特許番号
US07091362B2

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