HRID2352077

反应详情

EQUATION

反应方程式

HRID 2352077 的结构方程式

CONDITIONS

反应条件

温度
278 °C

PROCEDURE

实验过程

A 1 liter autoclave (316SS, Parr) was charged with 171 g (0.93 moles) isoflurane and 116 g (2.0 moles) potassium fluoride. The reaction mass was heated with stirring to 278° C. After 18 hours at 278° C., the pressure was 500 psi. The autoclave was then cooled to room temperature for transfer to the laboratory. Products were then distilled into a dry ice cooled trap by heating the autoclave on a hot plate. The trap contents (134 g) were distilled through a four foot vacuum jacketed column packed with glass beads to give 20.8 g CHF2OCHFCF3 (bp 23.5° C.). The material remaining in the distillation flask (104.0 g) was 98% isoflurane. Based on the materials isolated, the percent conversion was 13% (33% yield). Details of the distillation are given below.

WORKUP

后处理

  1. temperatureThe reaction mass was heated
  2. temperatureThe autoclave was then cooled to room temperature for transfer to the laboratory
  3. distillationProducts were then distilled into a dry ice cooled trap
  4. temperatureby heating the autoclave on a hot plate
  5. distillationThe trap contents (134 g) were distilled through a four foot vacuum