تفاعل #10020

ord-86800bf9397e44b882523bdaca98c2ce

المذيبات

ظروف التفاعل

درجة الحرارة
180°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىequipped with anchor stirrer
  2. 2
    درجة الحرارةthermometer, and reflux condenser
  3. 3
    أخرىwith bubble counter
  4. 4
    درجة الحرارةThe mixture was then heated
  5. 5
    درجة الحرارةthis temperature was maintained for 16 hours
  6. 6
    درجة الحرارةThe mixture was then cooled to room temperature
  7. 7
    workup.ADDITIONwater was added to the reaction mixture in a volumetric ratio of 1:1
  8. 8
    استخلاصthe mixture was extracted with diethyl ether
  9. 9
    غسيلAfter washing
  10. 10
    تركيزconcentration
  11. 11
    أخرىdrying the separated organic phase

الإجراء التجريبي

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%.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07091362B2uspto-grants-2006_08