Реакция #81693

Уравнение реакции

methanol

potassium hydroxide

C6F13I

→

C6F13H

Выход 98.1%

Растворители

water

Условия реакции

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
   ТемператураThe heating and refluxing
8. 8
   workup.WAITwere further continued for two hours
9. 9
   workup.DISSOLUTIONto dissolve
10. 10
    Другоеprecipitated potassium iodide
11. 11
    ДругоеThe crude reaction solution
12. 12
    Другоеwas separated into two layers
13. 13
    Промывкаthe fluorocarbon layer (lower layer) was further washed with 300 g of water
14. 14
    Другоеto recover the fluorocarbon

Методика

Into a 1 l four-necked flask equipped with a stirrer, a reflux condenser, a dropping funnel and a thermometer, 200 cc of methanol, 74.3 g (1.1 mols) of 85% potassium hydroxide and 1 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 the dropwise addition, heating and refluxing were continued for tow hours. The conversion at that time was 98.1%. The heating and refluxing were further continued for two hours. Then, the reactor was cooled to room temperature, and 200 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 the fluorocarbon. Thus, 157 g of C6F13H having a purity of 99.1%, was obtained.

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