反应详情

温度

130 °C

A mixed solution of 2 g of the above-mentioned 1,3,6-tribromopyrene, 2.5 g of 4-methylphenylboronic acid, 5.8 g of tripotassium phosphate, 0.88 g of tetrabutylammonium bromide, 61 mg of palladium acetate and 137 ml of deaerated dimethylformamide was heated while stirred under nitrogen gas stream at a temperature of 130° C. for 9 hours. After cooling the mixed solution to room temperature, 800 ml of water was injected thereinto to extract therefrom with 200 ml of dichloromethane. The organic layer was washed twice with 100 ml of water, dried by magnesium sulfate and thereafter concentrated by evaporation. The organic layer was purified by silica gel column chromatography and thereafter vacuum dried under a temperature of 70° C. to obtain 1.8 g of 1,3,6-tri(4-methylphenyl)pyrene as pale-yellow powder.

1. temperatureAfter cooling the mixed solution to room temperature
2. extractionto extract
3. washThe organic layer was washed twice with 100 ml of water
4. dry with materialdried by magnesium sulfate
5. concentrationconcentrated by evaporation
6. customThe organic layer was purified by silica gel column chromatography
7. customvacuum dried under a temperature of 70° C.