Реакция #81691

Уравнение реакции

C6F13I

methanol

isopropyl alcohol

potassium hydroxide

→

C6F13H

Выход 93.0%

Растворители

water

Условия реакции

Обработка

1. 1
   ТемператураThe reactor was heated
2. 2
   Другоеto 50° C
3. 3
   ТемператураWhile maintaining the internal temperature of the reactor at a level of from 50° to 55° C.
4. 4
   workup.WAITwas continued for 10 hours
5. 5
   workup.DISSOLUTIONto dissolve
6. 6
   Другоеprecipitated potassium iodide
7. 7
   ДругоеThe crude reaction solution
8. 8
   Другоеwas separated into two layers
9. 9
   Промывкаthe fluorocarbon layer (lower layer) was further washed twice with 3200 g of water

Методика

Into a 20 l Hastelloy C autoclave equipped with a stirrer, a reflux condenser and a thermometer, 5130 g of methanol and 60 g of isopropyl alcohol and 1485 g (22.5 mols) of 85% potassium hydroxide were charged. The reactor was heated to bring the internal temperature to 50° C. Then, 4460 g (10 mols) of C6F13I was fed thereto over a period of two hours. While maintaining the internal temperature of the reactor at a level of from 50° to 55° C. stirring was continued for 10 hours. The conversion was more than 99.9%. The reactor was cooled to room temperature, and then, 3200 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 twice with 3200 g of water to obtain 2975 g (purity: 99.9%) of C6F13H. In the reactor, no formation of tar was observed.

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