HRID622255

反应详情

EQUATION

反应方程式

HRID 622255 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
200 °C

PROCEDURE

实验过程

In an autoclave having an inner volume of 100 ml, 3.0 g (0.0126 mole) of 3,4,5,6-tetrafluorophthalic acid containing no sulfate ion, 0.5 g (0.0125 mole) of sodium hydroxide, and 50 g of water were placed and heated for reaction at 200° C. for 25 hours. After completion of the reaction, the reaction mixture was cooled to room temperature and extracted with 150 ml of diisopropyl ether. By analyzing this extract by gas chromatography using a 2 m column packed with SE52 and kept at 50° C., the reaction was found to have produced 2.9 mole % of 1,2,3,4-tetrafluorobenzene, 89.1 mole % of trifluorophenol, and substantially no 2,3,4,5-tetrafluorobenzoic acid based on the 3,4,5,6-tetrafluorophthalic acid used as the starting material [pH 2.75 at 25° C. at the time of charging].

WORKUP

后处理

  1. customAfter completion of the reaction
  2. temperaturethe reaction mixture was cooled to room temperature
  3. extractionextracted with 150 ml of diisopropyl ether
  4. extractionthis extract by gas chromatography
  5. customkept at 50° C.