反应详情

3.33 g (10 mmol) of 9-bromo-10-phenylanthracene was dissolved in 80 ml of tetrahydrofuran (abbreviation: THF), and the temperature was lowered to −78° C. 7.5 ml (12.0 mmol) of n-BuLi (1.6M) was dropped into the reaction solution by a dropping funnel, and it was stirred for 1 hour. A solution in which 5 g (20.0 mmol) of iodine was dissolved in 20 ml of THF was dropped and stirred for 2 hours at −78° C. After reaction, a sodium thiosulfate water solution was added to stop the reaction. An organic layer was washed with a sodium thiosulfate water solution and a saturated saline and dried with magnesium sulfate. After the natural filtration, the filtrate was concentrated and the obtained solid was recrystallized by ethanol. Then, 3.1 g of a light-yellow solid of 9-iodo-10-phenylanthracene, which was the intended object, was obtained with a yield of 83% (synthetic scheme of (b-5)).

1. customwas lowered to −78° C
2. additionwas dropped
3. stirringstirred for 2 hours at −78° C
4. customAfter reaction
5. customthe reaction
6. washAn organic layer was washed with a sodium thiosulfate water solution
7. dry with materiala saturated saline and dried with magnesium sulfate
8. filtrationAfter the natural filtration
9. concentrationthe filtrate was concentrated
10. customthe obtained solid was recrystallized by ethanol
11. customwas obtained with a yield of 83% (synthetic scheme of (b-5))