反应详情

温度

-78 °C

6.96 g of 9-(2-bromophenyl)-9H-carbazole as the intermediate of Preparation Example 8 was dissolved in 10 mL of purified tetrahydrofuran, and the resulting solution was cooled to −78° C. and 8.64 mL of butyllithium was slowly added dropwise. The mixture was stirred at the same temperature for 30 min, and 6.12 g of 4,4′-dibromobenzophenone was added. The mixture was stirred at the same temperature for 40 min and then further stirred at room temperature for an additional 3 hours. The reaction was terminated with aqueous ammonium chloride, and the reaction mixture was extracted with ethyl ether. The organic layer was dewatered using anhydrous magnesium sulfate, and the organic solvent was then removed. The resulting solid was dispersed in ethanol, stirred for one day, filtered, and vacuum dried, thus obtaining an intermediate material. The solid thus obtained was dispersed in 10 mL of acetic acid, and 10 drops of concentrated sulfuric acid were added, after which the mixture was refluxed for 4 hours. The resulting solid was filtered, washed with ethanol, and vacuum dried, yielding a 8,8-bis(4-bromophenyl)-8H-indolo[3,2,1-de]acridine compound.

1. stirringThe mixture was stirred at the same temperature for 40 min
2. stirringfurther stirred at room temperature for an additional 3 hours
3. customThe reaction was terminated with aqueous ammonium chloride
4. extractionthe reaction mixture was extracted with ethyl ether
5. customthe organic solvent was then removed
6. additionThe resulting solid was dispersed in ethanol
7. stirringstirred for one day
8. filtrationfiltered
9. customvacuum dried
10. customthus obtaining an intermediate material
11. customThe solid thus obtained
12. temperatureafter which the mixture was refluxed for 4 hours
13. filtrationThe resulting solid was filtered
14. washwashed with ethanol, and vacuum
15. customdried