반응 #68681

반응 방정식

2-bromo-9,9-dimethyl-9H-fluorene

phthalic anhydride

aluminum chloride

→

2-(7-bromo-9,9-dimethyl-9H-fluorene-2-carbonyl)benzoic acid

수율 82.0%

용매

dichloromethane

반응 조건

후처리

1. 1
   기타After the reaction was terminated
2. 2
   workup.DISTILLATIONdistilled water
3. 3
   workup.ADDITIONwas gradually added
4. 4
   추출the reaction solution was extracted with dichloromethane and 3 times
5. 5
   세척washed with distilled water
6. 6
   기타After solvent removal
7. 7
   workup.ADDITION)-containing vessel
8. 8
   세척washed
9. 9
   여과filtered
10. 10
    기타dried

실험 절차

2-bromo-9,9-dimethyl-9H-fluorene (40 g, 0.146 mol) and phthalic anhydride (23.8 g, 0.161 mol) were placed in a reaction vessel and dichloromethane (1 l) was added thereto. Then, aluminum chloride (29.2 g, 0.219 mol) was gradually added at 0° C., and the reaction mixture was stirred at room temperature for 12 hours. After the reaction was terminated, distilled water was gradually added, and the reaction solution was extracted with dichloromethane and 3 times washed with distilled water. After solvent removal, the resultant solid was placed in a hexane(2 l)-containing vessel, washed, filtered and dried to give 2-(7-bromo-9,9-dimethyl-9H-fluorene-2-carbonyl)benzoic acid (50.4 g, yield 82%).

출처