反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 130 °C
PROCEDURE
实验过程
A mixed solution of 2.3 g of 1-bromo-7-tert-butylpyrene, 1.1 g of phenylboronic acid, 3.8 g of tribasic potassium phosphate, 0.58 g of tetrabutylammonium bromide, 12 mg of palladium acetate, and 30 ml of dimethylformamide was then 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 thereto, and the mixture was extracted with 50 ml of dichloromethane. The organic layer was washed twice with 20 ml of water, dried over magnesium sulfate, and then evaporated. The resulting residue was purified by silica gel column chromatography and dried under vacuum to give 1.5 g of 7-tert-butyl-1-phenylpyrene.
WORKUP
后处理
- temperatureAfter the mixture was cooled to room temperature
- extractionthe mixture was extracted with 50 ml of dichloromethane
- washThe organic layer was washed twice with 20 ml of water
- dry with materialdried over magnesium sulfate
- customevaporated
- customThe resulting residue was purified by silica gel column chromatography
- customdried under vacuum