HRID1670056

反应详情

EQUATION

反应方程式

HRID 1670056 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixed solution of 3 g of 2-tert-butylpyrene (65% content), 50 ml of dichloromethane and 15 ml of methanol was then cooled to 0° C. under a nitrogen stream, and a solution of 3.3 g of benzyltrimethylammonium tribromide in 10 ml of dichloromethane was added dropwise to the mixed solution. After the mixed solution was stirred at room temperature for 2 hours, 50 ml of water was added thereto, and the mixture was extracted with 50 ml of dichloromethane. The organic layer was washed twice with 50 ml of water, dried over magnesium sulfate, and then evaporated. Ten ml of methanol was added to the resulting solid and stirred for 10 minutes, and then the solid was separated by filtration. Thereafter, 30 ml of hexane was further added to the solid and stirred for 30 minutes, and then the solid was separated by filtration. The solid was dried under vacuum to give 2.3 g of 1-bromo-7-tert-butylpyrene.

WORKUP

后处理

  1. extractionthe mixture was extracted with 50 ml of dichloromethane
  2. washThe organic layer was washed twice with 50 ml of water
  3. dry with materialdried over magnesium sulfate
  4. customevaporated
  5. additionTen ml of methanol was added to the resulting solid
  6. stirringstirred for 10 minutes
  7. customthe solid was separated by filtration
  8. additionThereafter, 30 ml of hexane was further added to the solid
  9. stirringstirred for 30 minutes
  10. customthe solid was separated by filtration
  11. customThe solid was dried under vacuum