تفاعل #10019

ord-3f9b2d5d03764f1a87b8b010a3ba32b6

المذيبات

ظروف التفاعل

درجة الحرارة
170°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 6 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
    أخرىthe 3-chloro-4-fluorobenzonitrile that precipitated
  9. 9
    أخرىwas isolated by filtration
  10. 10
    غسيلwashing
  11. 11
    أخرىdrying

الإجراء التجريبي

172 g of 3,4-dichlorobenzonitrile, 200 g of dimethylsulfoxide, 69.6 g of potassium fluoride, and 3.95 g of (N,N-dimethylimidazolidino)tris-(diethylamino)phosphazenium chloride were placed in a 1 liter four-neck flask equipped with anchor stirrer, thermometer, and reflux condenser with bubble counter. The mixture was then heated with stirring to 170° C. and this temperature was maintained for 6 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 3-chloro-4-fluorobenzonitrile that precipitated was isolated by filtration, washing, and drying. 3-Chloro-4-fluorobenzo-nitrile was obtained in a yield of 92% of theory.

المصدر

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