HRID1670058

反应详情

EQUATION

反应方程式

HRID 1670058 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 1.5 g of 7-tert-butyl-1-phenylpyrene, 25 ml of dichloromethane and 8 ml of methanol was then cooled to 0° C. under a nitrogen stream, and a solution of 1.7 g of benzyltrimethylammonium tribromide in 5 ml of dichloromethane was added dropwise to the mixed solution. After the mixed solution was stirred at room temperature for 2 hours, 20 ml of water was added thereto, and the mixture was extracted with 20 ml of dichloromethane. The organic layer was washed twice with 20 ml of water, dried over magnesium sulfate, and then evaporated. Ten ml of methanol was added to the resulting solid and allowed to stand overnight. The precipitated solid was separated by filtration and dried under vacuum to give 1.9 g of 1-bromo-7-tert-butyl-3-phenylpyrene.

WORKUP

后处理

  1. extractionthe mixture was extracted with 20 ml of dichloromethane
  2. washThe organic layer was washed twice with 20 ml of water
  3. dry with materialdried over magnesium sulfate
  4. customevaporated
  5. additionTen ml of methanol was added to the resulting solid
  6. waitto stand overnight
  7. customThe precipitated solid was separated by filtration
  8. customdried under vacuum