反应详情

温度

-78 °C

3.33 g (10 mmol) of 9-bromo-10-phenylanthracene was dissolved in 80 mL of tetrahydrofuran (abbreviation: THF), and cooled to −78° C. Then, in a reaction solution thereof, 7.5 mL (12.0 mmol) of n-buthyllithium (abbreviation: n-BuLi) (1.6 mol/L hexane solution) was dropped by a dropping funnel and then stirred for one hour. A solution in which 5 g (20.0 mmol) of iodine dissolved in 20 mL of THF was dropped therein, and the further stirred for 2 hours at −78° C. After reaction, a sodium thiosulfate aqueous solution was added therein and stirred. An organic layer was washed with a sodium thiosulfate aqueous solution and saturated saline, and then dried with magnesium sulfate. The mixture was filtrated naturally, then the filtrate was concentrated, and then recrystallized with ethanol, 3.1 g of 9-iodo-10-phenylanthracene that was a target substance was obtained as a light yellow solid at a yield of 83% (Synthesis scheme (b-3)).

1. additionwas dropped
2. stirringthe further stirred for 2 hours at −78° C
3. customAfter reaction
4. stirringstirred
5. washAn organic layer was washed with a sodium thiosulfate aqueous solution and saturated saline
6. dry with materialdried with magnesium sulfate
7. filtrationThe mixture was filtrated naturally
8. concentrationthe filtrate was concentrated
9. customrecrystallized with ethanol, 3.1 g of 9-iodo-10-phenylanthracene that
10. customwas obtained as a light yellow solid at a yield of 83% (Synthesis scheme (b-3))