Реакция #81698

Уравнение реакции

potassium tert-butoxide

C6F13I

→

C6F13H

Выход 94.4%

Условия реакции

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
   workup.ADDITIONwere charged
6. 6
   ТемператураThe reactor was heated
7. 7
   Другоеto 60° C
8. 8
   workup.ADDITIONAfter completion of the dropwise addition
9. 9
   Температураheating
10. 10
    Температураrefluxing
11. 11
    workup.WAITwere continued for one hour
12. 12
    workup.DISTILLATIONA fraction with a boiling point of up to 75° C. was recovered by distillation from the reactor
13. 13
    Промывкаfurther washed five times with 200 g of water

Методика

Into a 1 l four-necked flask equipped with a stirrer, a distillation apparatus-equipped reflux condenser, a dropping funnel and a thermometer, 400 cc of isopropyl alcohol (the water content in the isopropyl alcohol being not higher than 50 ppm, the same is true in the following Examples), and 84.2 g (0.75 mol) of potassium tert-butoxide 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 two hours. After completion of the dropwise addition, heating and refluxing were continued for one hour. The conversion at that time was 100%. A fraction with a boiling point of up to 75° C. was recovered by distillation from the reactor and further washed five times with 200 g of water, to obtain 151 g of C6F13H having a purity of 99.8%. In the reactor, no formation of tar was observed.

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