HRID53412

反应详情

EQUATION

反应方程式

HRID 53412 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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, 256 g of methanol, 3 g of isopropyl alcohol and 46.4 g (1.16 mol) of sodium hydroxide 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 the dropwise addition, heating and refluxing were continued for 6 hours. The conversion was more than 99.9%. The reactor was cooled to room temperature, and then, 300 g of water was added to dissolve precipitated sodium iodide. The crude reaction solution was separated into two layers, and the fluorocarbon layer (lower layer) was further washed twice with 300 g of water to obtain 145 g (purity: 99.9%) of C6F13H. 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, 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 6 hours
  8. dissolutionto dissolve
  9. customprecipitated sodium iodide
  10. customThe crude reaction solution
  11. customwas separated into two layers
  12. washthe fluorocarbon layer (lower layer) was further washed twice with 300 g of water