Reaktion #68681

Reaktionsgleichung

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

phthalic anhydride

aluminum chloride

→

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

Ausbeute 82.0%

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeAfter the reaction was terminated
2. 2
   workup.DISTILLATIONdistilled water
3. 3
   workup.ADDITIONwas gradually added
4. 4
   Extraktionthe reaction solution was extracted with dichloromethane and 3 times
5. 5
   Waschenwashed with distilled water
6. 6
   SonstigeAfter solvent removal
7. 7
   workup.ADDITION)-containing vessel
8. 8
   Waschenwashed
9. 9
   Filtrationfiltered
10. 10
    Sonstigedried

Vorschrift

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%).

Quelle