HRID1416324

反应详情

EQUATION

反应方程式

HRID 1416324 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Preparation of the sodium salt of 2,3,5,6-tetrafluoropyridine-4-thiol 4-Chloro-2,3,5,6-tetrafluoropyridine (2 g) and sodium hydrosulfide dihydrate were stirred and heated under reflux in iso-propanol (40 cm3) for 3 hours. The mixture was then stirred at the ambient temperature for 18 hours. The precipitated solid was removed by filtration, washed with diethyl ether and discarded. The combined organic solutions were evaporated under reduced pressure to give 2,3,5,6-tetrafluoropyridine-4-thiol as its sodium salt (2.21 g), which was used without further purification in the second step.

WORKUP

后处理

  1. temperatureheated
  2. stirringThe mixture was then stirred at the ambient temperature for 18 hours
  3. customThe precipitated solid was removed by filtration
  4. washwashed with diethyl ether
  5. customThe combined organic solutions were evaporated under reduced pressure