Реакция #81696

ord-170786d7e07c432a8a0b319eaf4533a6

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
    Температураreflux 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 3 hours
  11. 11
    workup.DISTILLATIONA fraction with a boiling point of up to 75° C. was recovered by distillation from the reactor
  12. 12
    ПромывкаThis recovered liquid was washed five times with 200 g of water, and acetone and isopropyl alcohol
  13. 13
    Другоеwere removed

Методика

Into a 1 l four-necked flask equipped with a stirrer, a distillation apparatus-equipped reflux condenser, a dropping funnel and a thermometer, 200 cc of isopropyl alcohol, 87.5 g (0.75 mol) of 48% potassium hydroxide and 1 g of tetrabutyl ammonium 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 3 hours. The conversion at that time was 99.9%. A fraction with a boiling point of up to 75° C. was recovered by distillation from the reactor. This recovered liquid was washed five times with 200 g of water, and acetone and isopropyl alcohol were removed. Thus, 146 g of C6F13H having a purity of 99.9%, was obtained.

Источник

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