反应详情

24.3 g (100 mmol) of 9-phenylcarbazole was put into a 2-L Erlenmeyer flask and dissolved by addition of 600 mL of glacial acetic acid. 17.8 g (100 mmol) of N-bromosuccinimide was slowly added into this solution and stirred for about 12 hours at room temperature. By dripping this reaction solution into 1 L of ice water while being stirred, a white solid was separated out. This separated white solid was recovered by suction filtration and washed three times with water. This solid was dissolved in 150 mL of diethyl ether and washed with a saturated sodium acid carbonate solution and water. This organic layer was dried with magnesium sulfate. Suction filtration of the mixture was performed, and the resulting filtrate was enriched. Recrystallization thereof was performed by addition of about 50 mL of methanol into this enriched solution and being left standing, whereby 28.4 g of a white powder solid of 3-bromo-9-phenylcarbazole was obtained at a yield of 88%.

1. stirringwhile being stirred
2. customa white solid was separated out
3. filtrationThis separated white solid was recovered by suction filtration
4. washwashed three times with water
5. dissolutionThis solid was dissolved in 150 mL of diethyl ether
6. washwashed with a saturated sodium acid carbonate solution and water
7. dry with materialThis organic layer was dried with magnesium sulfate
8. filtrationSuction filtration of the mixture
9. customRecrystallization
10. additionthereof was performed by addition of about 50 mL of methanol into this enriched solution
11. waitbeing left standing, whereby 28.4 g of a white powder solid of 3-bromo-9-phenylcarbazole
12. customwas obtained at a yield of 88%