Реакция #81692

ord-54f8a64d08b74411b846a4c35d500602

Растворители

Условия реакции

Температура
55°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураThe reactor was heated
  2. 2
    Другоеto 55° C
  3. 3
    workup.WAITwas continued for 10 hours
  4. 4
    workup.DISSOLUTIONto dissolve
  5. 5
    Другоеprecipitated potassium iodide
  6. 6
    ДругоеThe crude reaction solution
  7. 7
    Другоеwas separated into two layers
  8. 8
    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, a dropping funnel and a thermometer, 7700 g of methanol, 60 g of isopropyl alcohol and 1980 g (30 mols) of 85% potassium hydroxide were charged. The reactor was heated to bring the internal temperature to 55° C. Then, 4460 g (10 mols) of C6F13I was fed thereto over a period of two hours. While maintaining the reactor at 55° C. stirring was continued for 10 hours. The conversion was more than 99.9%. 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 2951 g of C6F13H (purity: 99.9%, 3.9 ppm of C6F13I was detected). In the reactor, no formation of tar was observed.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05618986uspto-grants-1997_04