反应详情

温度

130 °C

Next, a mixed solution of 2.0 g of 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 with stirring under a nitrogen gas flow at 130° C. for 9 hours. After cooling to room temperature, 800 ml of water was injected, followed by extraction with 200 ml of dichloromethane. The organic layer was washed twice with 100 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 1.8 g of 1,3,6-tri(4-methylphenyl)pyrene as a pale yellow powder.

1. temperatureAfter cooling to room temperature
2. extractionfollowed by extraction with 200 ml of dichloromethane
3. washThe organic layer was washed twice with 100 ml of water
4. dry with materialdried over magnesium sulfate
5. customevaporated
6. concentrationThe resultant concentrate
7. customwas purified by silica gel column chromatography
8. customvacuum-dried