HRID53420

反应详情

EQUATION

反应方程式

HRID 53420 的结构方程式

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. customInto a 1 l four-necked flask equipped with a stirrer
  2. distillationa distillation
  3. customapparatus-equipped
  4. temperaturereflux condenser, a dropping funnel
  5. additionwere charged
  6. temperatureThe reactor was heated
  7. customto 60° C
  8. additionAfter completion of the dropwise addition
  9. temperatureheating
  10. temperaturerefluxing
  11. waitwere continued for one hour
  12. distillationA fraction with a boiling point of up to 75° C. was recovered by distillation from the reactor
  13. washfurther washed five times with 200 g of water