Реакция #81690

Уравнение реакции

C6F13I

methanol

isopropyl alcohol

sodium hydroxide

→

C6F13H

Выход 90.6%

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
   workup.WAITwere continued for 6 hours
8. 8
   workup.DISSOLUTIONto dissolve
9. 9
   Другоеprecipitated sodium iodide
10. 10
    ДругоеThe crude reaction solution
11. 11
    Другоеwas separated into two layers
12. 12
    Промывкаthe fluorocarbon layer (lower layer) was further washed twice with 300 g of water

Методика

Into a 1 l four-necked flask equipped with a stirrer, a reflux condenser, a dropping funnel and a thermometer, 256 g of methanol, 3 g of isopropyl alcohol and 46.4 g (1.16 mol) of sodium hydroxide 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 6 hours. The conversion was more than 99.9%. The reactor was cooled to room temperature, and then, 300 g of water was added to dissolve precipitated sodium iodide. The crude reaction solution was separated into two layers, and the fluorocarbon layer (lower layer) was further washed twice with 300 g of water to obtain 145 g (purity: 99.9%) of C6F13H. In the reactor, no formation of tar was observed.

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