HRID1289114

反应详情

EQUATION

反应方程式

HRID 1289114 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

0.55 g of 5-formyl-2,2'-bithiophene was dissolved in 10 ml of dichloromethane. 1.95 g of PPh3 and 1.23 g of CBr4 were dissolved in 40 ml of dichloromethane and mixed with the 5-formyl-2,2'-bithiophene/dichloromethane solution under nitrogen gas atmosphere at 0° C. After the mixture was stirred for 1 hour and 10 ml of n-hexane was added to precipitate the triphenyl-phosphine oxide. And the reaction solution was filtered. Further, 100 ml of n-hexane was then added into the solution and the yellowish solid was obtained. The solid was further purified by column chromatography and crystallized with ethanol. The crystal product was thus obtained and the melting point thereof was 112°-113° C.

WORKUP

后处理

  1. customto precipitate the triphenyl-phosphine oxide
  2. filtrationAnd the reaction solution was filtered
  3. additionFurther, 100 ml of n-hexane was then added into the solution
  4. customthe yellowish solid was obtained
  5. customThe solid was further purified by column chromatography
  6. customcrystallized with ethanol
  7. customThe crystal product was thus obtained
  8. customthereof was 112°-113° C.