HRID1404883

反应详情

EQUATION

反应方程式

HRID 1404883 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

Then, a mixed solution of 2.3 g (content 79.2%) of 1-bromo-7-t-butylpyrene, 1.1 g of phenylboronic acid, 3.8 g of tripotassium phosphate, 0.58 g of tetrabutylammonium bromide, 12 mg of palladium acetate and 30 ml of dimethylformamide was heated and stirred at 130° C. for 2 hours under a nitrogen stream. After the mixture was cooled to room temperature, 30 ml of water was added, and this was extracted with 50 ml of dichloromethane. The organic layer was washed with 20 ml of water two times, dried with magnesium sulfate, and evaporated. This was purified by silica gel column chromatography, and vacuum-dried to obtain 1.5 g of 7-t-butyl-1-phenylpyrene.

WORKUP

后处理

  1. temperatureAfter the mixture was cooled to room temperature
  2. extractionthis was extracted with 50 ml of dichloromethane
  3. washThe organic layer was washed with 20 ml of water two times
  4. dry with materialdried with magnesium sulfate
  5. customevaporated
  6. customThis was purified by silica gel column chromatography
  7. customvacuum-dried