HRID1914413

反应详情

EQUATION

反应方程式

HRID 1914413 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Next, a mixed solution of 3 g (content: 65%) of 2-t-butylpyrene, 50 ml of dichloromethane and 15 ml of methanol was cooled to 0° C. under a nitrogen gas stream and then 3.3 g of benzyltrimethylammonium tribromide dissolved in 10 ml of dichloromethane was added dropwise. This mixed solution was stirred at room temperature for 2 hours and 50 ml of water was poured into the solution, followed by extraction with 50 ml of dichloromethane. The organic layer was washed twice with 50 ml of water, dried over magnesium sulfate and then evaporated. To the resulting solid, 10 ml of methanol was added, followed by stirring for 10 minutes and further filtration. Furthermore, 30 ml of hexane was added and, after stirring for 30 minutes, the solution was filtered and the filtrate was vacuum-dried to obtain 2.3 g of 1-bromo-7-t-butylpyrene.

WORKUP

后处理

  1. additionwas added dropwise
  2. extractionfollowed by extraction with 50 ml of dichloromethane
  3. washThe organic layer was washed twice with 50 ml of water
  4. dry with materialdried over magnesium sulfate
  5. customevaporated
  6. additionTo the resulting solid, 10 ml of methanol was added
  7. stirringby stirring for 10 minutes
  8. filtrationfurther filtration
  9. additionFurthermore, 30 ml of hexane was added
  10. stirringafter stirring for 30 minutes
  11. filtrationthe solution was filtered
  12. customthe filtrate was vacuum-dried