HRID1670054

反应详情

EQUATION

反应方程式

HRID 1670054 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A mixed solution of 40 g of 1-(4-methylphenyl)pyrene, 24.4 g of N-bromosuccinimide and 1.4 l of dimethylformamide was then heated and stirred at 40° C. for 7 hours under a nitrogen stream. After the mixture was cooled to room temperature, 1 l (liter) of water was added thereto, and the mixture was extracted with 500 ml of dichloromethane. The organic layer was washed twice with 200 ml of water, dried over magnesium sulfate, and then filtered through celite. The filtrate was evaporated, and the resulting residue was washed twice with 200 ml of ethyl acetate. The precipitated solid was separated by filtration and dried under vacuum to give 11.4 g of 1-bromo-6-(4-methylphenyl)pyrene.

WORKUP

后处理

  1. temperatureAfter the mixture was cooled to room temperature
  2. extractionthe mixture was extracted with 500 ml of dichloromethane
  3. washThe organic layer was washed twice with 200 ml of water
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered through celite
  6. customThe filtrate was evaporated
  7. washthe resulting residue was washed twice with 200 ml of ethyl acetate
  8. customThe precipitated solid was separated by filtration
  9. customdried under vacuum