HRID1404882

反应详情

EQUATION

反应方程式

HRID 1404882 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Then, 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 stream, and 3.3 g of benzyltrimethylammonium tribromide dissolved in 10 ml of dichloromethane was added dropwise. After this mixed solution was stirred at room temperature for 2 hours, 50 ml of water was added, and this was extracted with 50 ml of dichloromethane. The organic layer was washed with 50 ml of water two times, dried with magnesium sulfate, and evaporated. To the resulting solid was added 10 ml of methanol, and the mixture was stirred for 10 minutes, and filtered. Further, 30 ml of hexane was added, and the mixture was stirred for 30 minutes, and filtered. After the resultant was vacuum dried, 2.3 g of 1-bromo-7-t-butylpyrene was obtained.

WORKUP

后处理

  1. additionwas added dropwise
  2. extractionthis was extracted with 50 ml of dichloromethane
  3. washThe organic layer was washed with 50 ml of water two times
  4. dry with materialdried with magnesium sulfate
  5. customevaporated
  6. additionTo the resulting solid was added 10 ml of methanol
  7. stirringthe mixture was stirred for 10 minutes
  8. filtrationfiltered
  9. additionFurther, 30 ml of hexane was added
  10. stirringthe mixture was stirred for 30 minutes
  11. filtrationfiltered
  12. customdried