HRID1914414
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
Next, a mixed solution of 2.3 g 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 under a nitrogen gas stream at 130° C. for 2 hours. The solution was cooled to room temperature and 30 ml of water was poured into the solution, followed by extraction with 50 ml of dichloromethane. The organic layer was washed twice with 20 ml of water, dried over magnesium sulfate and then evaporated. The concentrate was purified by silica gel column chromatography and then vacuum-dried to obtain 1.5 g of 7-t-butyl-1-phenylpyrene.
WORKUP
后处理
- temperatureThe solution was cooled to room temperature
- extractionfollowed by extraction with 50 ml of dichloromethane
- washThe organic layer was washed twice with 20 ml of water
- dry with materialdried over magnesium sulfate
- customevaporated
- customThe concentrate was purified by silica gel column chromatography
- customvacuum-dried