反应详情

9,9-Dimethyl-9H-fluorene (40 g, 1 eq, 0.146 mol) and phthalic anhydride (36.5 g, 1.1 eq, 0.161 mol) were placed in a reaction vessel, and dichloromethane (1.5 l) was added thereto. Then, aluminum chloride (29.2 g, 1.5 eq, 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 at 0° C., and the resultant solution was extracted with an excess of dichloromethane and several 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-(9,9-dimethyl-9H-fluorene-2-carbonyl)benzoic acid (59.8 g, yield=82%).

1. customAfter the reaction was terminated
2. distillationdistilled water
3. additionwas gradually added at 0° C.
4. extractionthe resultant solution was extracted with an excess of dichloromethane and several times
5. washwashed with distilled water
6. customAfter solvent removal
7. addition)-containing vessel
8. washwashed
9. filtrationfiltered
10. customdried