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
- 100 °C
PROCEDURE
实验过程
Next, a mixed solution of 4.6 g of 1-bromo-6-(4-methylphenyl)pyrene, 4.9 g of 2-(3-t-butylphenyl)-4,4,5,5-tetramethyl 1,3,2-dioxaborolane, 8.0 g of tripotassium phosphate, 306 mg of PdCl2(dppf).CH2Cl2 and 75 ml of deaerated dimethylformamide was heated with stirring under a nitrogen gas flow at 100° C. for 6 hours. After cooling to room temperature, 100 ml of water was injected, followed by extraction with 100 ml of dichloromethane. The organic layer was washed twice with 50 ml of water, dried over magnesium sulfate and then evaporated. The resultant concentrate was purified by silica gel column chromatography and then vacuum-dried to obtain 4.3 g of 1-(3-t-butylphenyl)-6-(4-methylphenyl)pyrene.
WORKUP
后处理
- temperatureAfter cooling to room temperature
- extractionfollowed by extraction with 100 ml of dichloromethane
- washThe organic layer was washed twice with 50 ml of water
- dry with materialdried over magnesium sulfate
- customevaporated
- concentrationThe resultant concentrate
- customwas purified by silica gel column chromatography
- customvacuum-dried