HRID522307

反应详情

EQUATION

反应方程式

HRID 522307 的结构方程式

CONDITIONS

反应条件

温度
240 °C

PROCEDURE

实验过程

C4F9CH2CF2CH2CH2OH was produced by introducing ethylene (25 g, 0.53 mol) was introduced to an autoclave charged with C4F9CH2CF2I (217 g, 0.87 mol) and d-(+)-limonene (1 g), and then the reactor was heated at 240° C. for 12 hours. Product was obtained via vacuum distillation 81˜91° C. at 19˜24 mmHg in 62% yield. Fuming sulfuric acid (70 mL) was added slowly to 50 g of C4F9CH2CF2CH2CH2I and mixture was stirred at 60° C. for 1.5 h. The reaction was quenched with ice-cold 1.5 wt % Na2SO3 aqueous solution and heated at 95° C. for 0.5 h. The bottom layer was separated and washed with 10 wt % aqueous sodium acetate and distilled to provide compound of formula C4F9CH2CF2CH2CH2OH: by 54-57° C. at 2 mmHg (267 Pascals).

WORKUP

后处理

  1. additionwas introduced to an autoclave
  2. customProduct was obtained via vacuum distillation 81˜91° C. at 19˜24 mmHg in 62% yield
  3. customThe reaction was quenched with ice-cold 1.5 wt % Na2SO3 aqueous solution
  4. temperatureheated at 95° C. for 0.5 h
  5. customThe bottom layer was separated
  6. washwashed with 10 wt % aqueous sodium acetate
  7. distillationdistilled