HRID1251530

反应详情

EQUATION

反应方程式

HRID 1251530 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a THF (30 ml) solution including 5.0 g (18.6 mmol) of 2,7-di-tert-butylfluorene, a hexane solution (13.5 ml, 21.6 mmol) of n-butyllithium was added dropwise at −78° C. under nitrogen, followed by stirring at room temperature for 6 hours. Next, a THF (20 ml) solution including 3.42 g (23.4 mmol) of cyclohexylfulvene was added dropwise at 0° C. under a nitrogen atmosphere, followed by stirring at room temperature for 16 hours. The resultant reaction solution was decomposed with cold water, and then extracted with ether. The extract was dried over magnesium sulfate and then filtered, and the used solvent was removed from the filtrate under reduced pressure, thereby obtaining a solid. This solid was recrystallized from methanol to obtain 5.36 g of a colorless solid.

WORKUP

后处理

  1. additionwas added dropwise at 0° C. under a nitrogen atmosphere
  2. stirringby stirring at room temperature for 16 hours
  3. customThe resultant reaction solution
  4. extractionextracted with ether
  5. dry with materialThe extract was dried over magnesium sulfate
  6. filtrationfiltered
  7. customthe used solvent was removed from the filtrate under reduced pressure
  8. customobtaining a solid
  9. customThis solid was recrystallized from methanol