Реакция #81694

ord-58ac287d8cc14b7892f4b6e9a504f375

Уравнение реакции

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеInto a 1 l four-necked flask equipped with a stirrer
  2. 2
    workup.DISTILLATIONa distillation
  3. 3
    Другоеapparatus-equipped
  4. 4
    Температураrefluxing condenser, a dropping funnel
  5. 5
    ТемператураThe reactor was heated
  6. 6
    Другоеto 60° C
  7. 7
    workup.ADDITIONAfter completion of dropwise addition
  8. 8
    Температураheating
  9. 9
    Температураrefluxing
  10. 10
    workup.WAITwere continued for two hours
  11. 11
    workup.DISTILLATIONA fraction with a boiling point of up to 60° C. was recovered by distillation from the reactor
  12. 12
    ПромывкаThe recovered liquid was washed with 300 g of water
  13. 13
    Другоеto recover the fluorocarbon

Методика

Into a 1 l four-necked flask equipped with a stirrer, a distillation apparatus-equipped refluxing condenser, a dropping funnel and a thermometer, 200 cc of methanol, 131 g of (1.1 mols) of 48% potassium hydroxide and 3 g of tetrabutylphosphonium bromide were charged. The reactor was heated to bring the internal temperature to 60° C. Then, 223 g (0.5 mol) of C6F13I was dropwise added thereto over a period of one hour. After completion of dropwise addition, heating and refluxing were continued for two hours. The conversion at that time was 97.0%. A fraction with a boiling point of up to 60° C. was recovered by distillation from the reactor. The recovered liquid was washed with 300 g of water to recover the fluorocarbon. Thus, 149 g of C6F13H having a purity of 99.9%, was obtained.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05618986uspto-grants-1997_04