反应详情

After 14 ml of THF was added to 678 mg of 2-bromo-3-iodo-6,7-didodecylanthraquinone obtained in the above and the compound was dissolved therein, 2.7 ml (2.7 mmol) of a toluene solution of diisopropylaluminum hydride (manufactured by Kanto Chemical Co., Ltd., 0.99M) was added, followed by 2 hours of stirring at room temperature. After ice cooling, 5 ml of 6N hydrochloric acid was added and then the mixture was heated to 65° C., followed by 4 hours of reaction. Toluene and an aqueous sodium chloride solution were added thereto and phase separation was conducted. Further, after washing with an aqueous sodium chloride solution, the organic phase was concentrated under reduced pressure and dried under vacuum. The obtained residue was again subjected to repeated reduction with diisopropylaluminum hydride and dehydration operation with 6N hydrochloric acid. The crude product was purified by recrystallization from toluene to obtain 469 mg of 2-bromo-3-iodo-6,7-didodecylanthracene as a light yellow solid (yield 72%).

1. customobtained in the above and the compound
2. dissolutionwas dissolved
3. temperaturethe mixture was heated to 65° C.
4. customfollowed by 4 hours of reaction
5. customphase separation
6. washFurther, after washing with an aqueous sodium chloride solution
7. concentrationthe organic phase was concentrated under reduced pressure
8. customdried under vacuum
9. customThe crude product was purified by recrystallization from toluene