Reacción #81697

Ecuación de reacción

C8F17I

methanol

potassium hydroxide

→

C8F17H

Rendimiento 93.8%

Disolventes

water

Condiciones de reacción

Tratamiento posterior

1. 1
   OtroInto a 1 l four-necked flask equipped with a stirrer, a reflux condenser, a dropping funnel
2. 2
   TemperaturaThe reactor was heated
3. 3
   Otroto 60° C
4. 4
   workup.ADDITIONAfter completion of the dropwise addition
5. 5
   Temperaturaheating
6. 6
   Temperaturarefluxing
7. 7
   workup.WAITwere continued for 8 hours
8. 8
   workup.DISSOLUTIONto dissolve
9. 9
   Otroprecipitated potassium iodide
10. 10
    OtroThe crude reaction solution
11. 11
    Otrowas separated into two layers
12. 12
    Lavadothe fluorocarbon layer (lower layer) was further washed with 300 g of water
13. 13
    Otroto recover a fluorocarbon

Procedimiento

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.

Fuente