反应详情

温度

-78 °C

10 g (24 mmol) of 2-bromo-9,10-diphenylanthracene was put into a 500 mL three-neck flask, the atmosphere in the flask was substituted with nitrogen, and then 150 mL of tetrahydrofuran was added thereto and dissolved well. This solution was stirred at −78° C. 19 mL of n-butyllithium solution (1.6 mmol/L) was dropped into this solution with a syringe and the mixture was stirred at −78° C. for one hour, so that a white solid substance was precipitated. After reaction, a solution in which 12 g (49 mmol) of iodine was dissolved into 80 mL of tetrahydrofuran was dropped into this reacted mixture with use of a dropping funnel. After the dropping, the mixture was stirred at −78° C. for one hour and at room temperature for 12 hours. After reaction, a sodium thiosulfate solution was added into the reaction solution, and was stirred at room temperature for one hour. Ethyl acetate was added into this mixture for extraction. An aqueous layer and an organic layer were separated, and the organic layer was washed with sodium thiosulfate solution and saturated saline in this order. The aqueous layer and the organic layer were separated and the organic layer was dried with magnesium sulfate. This mixture was suction-filtrated to remove the magnesium sulfate. The obtained filtrate was concentrated, so that a solid substance was obtained. Methanol was added into this solid substance and washed by ultrasonic wave irradiation, so that a solid substance was precipitated. This solid substance was collected by suction filtration, so that 9.9 g of a light yellow powdered solid substance was obtained in a yield of 90%.

1. dissolutiondissolved well
2. stirringthe mixture was stirred at −78° C. for one hour, so that a white solid substance
3. customwas precipitated
4. customAfter reaction
5. additionwas dropped into this reacted mixture with use of a dropping funnel
6. stirringAfter the dropping, the mixture was stirred at −78° C. for one hour and at room temperature for 12 hours
7. customAfter reaction
8. stirringwas stirred at room temperature for one hour
9. customAn aqueous layer and an organic layer were separated
10. washthe organic layer was washed with sodium thiosulfate solution and saturated saline in this order
11. customThe aqueous layer and the organic layer were separated
12. dry with materialthe organic layer was dried with magnesium sulfate
13. filtrationThis mixture was suction-filtrated
14. customto remove the magnesium sulfate
15. concentrationThe obtained filtrate was concentrated, so that a solid substance
16. customwas obtained
17. washwashed by ultrasonic wave irradiation, so that a solid substance
18. customwas precipitated
19. filtrationThis solid substance was collected by suction filtration, so that 9.9 g of a light yellow powdered solid substance
20. customwas obtained in a yield of 90%