反应详情

To a 100 ml three-necked flask were added 1.00 g (2.83=mol) of 4-bromo-5-iodophthalic anhydride synthesized in the above, 1.29 g (3.11 mmol) of 1,2-didodecylbenzene, and 4 ml of tetrachloroethane. Thereto was added 0.82 g (6.15 mmol) of aluminum chloride, followed by 3 hours of stirring at room temperature. Ice was added portionwise to the resulting reaction mixture to quench the reaction, followed by extraction with toluene. The extract was concentrated under reduced pressure to obtain 2.5 g of a viscous matter. To the viscous matter was added 8 ml of sulfuric acid, followed by 2 hours of stirring at 80° C. The resulting reaction mixture was cooled to room temperature and ice was added. The mixture was extracted with toluene and the organic phase was dried over sodium sulfate. Then, the phase was filtrated and concentrated under reduced pressure to obtain 678 mg of 2-bromo-3-iodo-6,7-didodecylanthraquinone (yield 35%).

1. additionIce was added portionwise to the resulting reaction mixture
2. customto quench
3. customthe reaction
4. extractionfollowed by extraction with toluene
5. concentrationThe extract was concentrated under reduced pressure
6. customto obtain 2.5 g of a viscous matter
7. waitfollowed by 2 hours
8. stirringof stirring at 80° C
9. customThe resulting reaction mixture
10. temperaturewas cooled to room temperature
11. additionice was added
12. extractionThe mixture was extracted with toluene
13. dry with materialthe organic phase was dried over sodium sulfate
14. filtrationThen, the phase was filtrated
15. concentrationconcentrated under reduced pressure