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
PROCEDURE
实验过程
Next, a mixed solution of 3 g (content: 65%) of 2-t-butylpyrene, 50 ml of dichloromethane and 15 ml of methanol was cooled to 0° C. under a nitrogen gas stream and then 3.3 g of benzyltrimethylammonium tribromide dissolved in 10 ml of dichloromethane was added dropwise. This mixed solution was stirred at room temperature for 2 hours and 50 ml of water was poured into the solution, followed by extraction with 50 ml of dichloromethane. The organic layer was washed twice with 50 ml of water, dried over magnesium sulfate and then evaporated. To the resulting solid, 10 ml of methanol was added, followed by stirring for 10 minutes and further filtration. Furthermore, 30 ml of hexane was added and, after stirring for 30 minutes, the solution was filtered and the filtrate was vacuum-dried to obtain 2.3 g of 1-bromo-7-t-butylpyrene.
WORKUP
后处理
- additionwas added dropwise
- extractionfollowed by extraction with 50 ml of dichloromethane
- washThe organic layer was washed twice with 50 ml of water
- dry with materialdried over magnesium sulfate
- customevaporated
- additionTo the resulting solid, 10 ml of methanol was added
- stirringby stirring for 10 minutes
- filtrationfurther filtration
- additionFurthermore, 30 ml of hexane was added
- stirringafter stirring for 30 minutes
- filtrationthe solution was filtered
- customthe filtrate was vacuum-dried