HRID53419

反应详情

EQUATION

反应方程式

HRID 53419 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. customInto a 1 l four-necked flask equipped with a stirrer, a reflux condenser, a dropping funnel
  2. temperatureThe reactor was heated
  3. customto 60° C
  4. additionAfter completion of the dropwise addition
  5. temperatureheating
  6. temperaturerefluxing
  7. waitwere continued for 8 hours
  8. dissolutionto dissolve
  9. customprecipitated potassium iodide
  10. customThe crude reaction solution
  11. customwas separated into two layers
  12. washthe fluorocarbon layer (lower layer) was further washed with 300 g of water
  13. customto recover a fluorocarbon