HRID53416

反应详情

EQUATION

反应方程式

HRID 53416 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 distillation apparatus-equipped refluxing condenser, a dropping funnel and a thermometer, 200 cc of methanol, 131 g of (1.1 mols) of 48% potassium hydroxide and 3 g of tetrabutylphosphonium bromide 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 one hour. After completion of dropwise addition, heating and refluxing were continued for two hours. The conversion at that time was 97.0%. A fraction with a boiling point of up to 60° C. was recovered by distillation from the reactor. The recovered liquid was washed with 300 g of water to recover the fluorocarbon. Thus, 149 g of C6F13H having a purity of 99.9%, was obtained.

WORKUP

后处理

  1. customInto a 1 l four-necked flask equipped with a stirrer
  2. distillationa distillation
  3. customapparatus-equipped
  4. temperaturerefluxing condenser, a dropping funnel
  5. temperatureThe reactor was heated
  6. customto 60° C
  7. additionAfter completion of dropwise addition
  8. temperatureheating
  9. temperaturerefluxing
  10. waitwere continued for two hours
  11. distillationA fraction with a boiling point of up to 60° C. was recovered by distillation from the reactor
  12. washThe recovered liquid was washed with 300 g of water
  13. customto recover the fluorocarbon