Реакция #81697

ord-c651a9626b3742698ca1704d02ec5745

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеInto a 1 l four-necked flask equipped with a stirrer, a reflux condenser, a dropping funnel
  2. 2
    ТемператураThe reactor was heated
  3. 3
    Другоеto 60° C
  4. 4
    workup.ADDITIONAfter completion of the dropwise addition
  5. 5
    Температураheating
  6. 6
    Температураrefluxing
  7. 7
    workup.WAITwere continued for 8 hours
  8. 8
    workup.DISSOLUTIONto dissolve
  9. 9
    Другоеprecipitated potassium iodide
  10. 10
    ДругоеThe crude reaction solution
  11. 11
    Другоеwas separated into two layers
  12. 12
    Промывкаthe fluorocarbon layer (lower layer) was further washed with 300 g of water
  13. 13
    Другоеto recover a fluorocarbon

Методика

Into a 1 l four-necked flask equipped with a stirrer, a reflux condenser, a dropping funnel and a thermometer, 250 cc of methanol and 3 g of tetrabutylphosphonium bromide and 74.3 g (1.1 mols) of 85% potassium hydroxide were charged. The reactor was heated to bring the internal temperature to 60° C. Then, 273 g (0.5 mol) of C8F17I was dropwise added thereto over a period of one hour. After completion of the dropwise addition, heating and refluxing were continued for 8 hours. The conversion at that time was 99.6%. The reactor was cooled to room temperature. Then, 300 g of water was added to dissolve precipitated potassium iodide. The crude reaction solution was separated into two layers, and the fluorocarbon layer (lower layer) was further washed with 300 g of water to recover a fluorocarbon. Thus, 197 g of C8F17H having a purity of 99.0%, was obtained.

Источник

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