HRID1907172

反应详情

EQUATION

反应方程式

HRID 1907172 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into a 300 ml three-necked glass flask equipped with a thermometer, a reflux condenser and a stirrer, 3,5-dichloroiodobenzene 22.6 g (82.8 mmol) and dimethylformamide 200 ml were added, and argon was passed through the solution for 2 hours and 15 minutes. Then, 3,5-dichlorothiophenol 14.8 g (82.6 mmol), potassium carbonate 22.8 g (165 mmol) and cuprous iodide 1.57 g (8.24 mmol) were added, which were reacted for 3 hours at 95 to 100° C. with stirring. After completion of the reaction, the reaction mixture was cooled down to room temperature and separated with the addition of water and hexane:ethyl acetate (1:1), and the organic layer obtained was dried with anhydrous magnesium sulfate. After filtration, the filtrate was concentrated under reduced pressure, and the obtained concentrate was purified by recrystallization, simple silica-gel column chromatography (eluent; hexane) to obtain bis(3,5-dichlorophenyl)sulfide 25.4 g as white solid (isolation yield; 95%).

WORKUP

后处理

  1. additionwere added
  2. customwhich were reacted for 3 hours at 95 to 100° C.
  3. customAfter completion of the reaction
  4. customseparated with the addition of water and hexane:ethyl acetate (1:1)
  5. customthe organic layer obtained
  6. dry with materialwas dried with anhydrous magnesium sulfate
  7. filtrationAfter filtration
  8. concentrationthe filtrate was concentrated under reduced pressure
  9. concentrationthe obtained concentrate
  10. customwas purified by recrystallization, simple silica-gel column chromatography (eluent; hexane)