HRID963782

反应详情

EQUATION

反应方程式

HRID 963782 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a three-necked flask provided with a stirring device, a reflux condenser, and a thermometer, 13.90 g (66 m.mols) of pentafluorobenzoic acid, 40 g of ethylene glycol, and 0.82 g (11 m.mols) of calcium hydroxide were placed and heated and the ensuant reaction was continued for 6 hours, with the reaction temperature gradually lowered meanwhile from the initial level of 140° C. to the terminal level of 110° C. After the reaction was completed, pentafluorobenzene was isolated by distillation. By the distillation, pentafluorobenzene was obtained in an amount of 8.02 g (48 m.mols), i.e. in a yield of 72.8%. By gas chromatography, the product was found to have purity of not less than 99.0%. The solution remaining after the distillation could be recycled through the subsequent cycle of reaction, though the pentafluorobenzoic acid as the starting material remained in the solution.

WORKUP

后处理

  1. customIn a three-necked flask provided with a stirring device, a reflux condenser
  2. temperatureheated
  3. customthe ensuant reaction
  4. customlevel of 140° C.
  5. customto the terminal level of 110° C