反应详情

温度

120 °C

8.32 (17.3 mmol) of 2-bromo-9,10-bis(4-fluorophenyl)-9,10-dihydro-9,10-anthracenediol, 5.17 g (31.1 mmol) of potassium iodide, 9.90 g (93.4 mmol) of sodium phosphinate monohydrate, and 50 mL of glacial acetic acid were put into a 200 mL three-neck flask, and the mixture was refluxed at 120° C. for 4 hours. Then, 20 mL of a 50% phosphinic acid was added into the reaction mixture, and the mixture was stirred for 1 hour at 120° C. After the reaction, the reaction mixture was washed with water, and the aqueous layer was extracted with ethyl acetate. This extracted solution was combined with the organic layer, and then dried with magnesium sulfate. After drying, the mixture was subjected to suction filtration, and the filtrate was concentrated. The obtained residue was dissolved in toluene, and filtered through Florisil, celite, and then alumina, and the filtrate was concentrated. The obtained residue was recrystallized with chloroform and hexane, giving 7.2 g of 2-bromo-9,10-bis(4-fluorophenyl)anthracene as light yellow powder in 74% yield.

1. customAfter the reaction
2. washthe reaction mixture was washed with water
3. extractionthe aqueous layer was extracted with ethyl acetate
4. dry with materialdried with magnesium sulfate
5. customAfter drying
6. filtrationthe mixture was subjected to suction filtration
7. concentrationthe filtrate was concentrated
8. dissolutionThe obtained residue was dissolved in toluene
9. filtrationfiltered through Florisil, celite
10. concentrationalumina, and the filtrate was concentrated
11. customThe obtained residue was recrystallized with chloroform and hexane