تفاعل #68681

معادلة التفاعل

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

phthalic anhydride

aluminum chloride

→

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

المردود 82.0%

المذيبات

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   أخرىAfter the reaction was terminated
2. 2
   workup.DISTILLATIONdistilled water
3. 3
   workup.ADDITIONwas gradually added
4. 4
   استخلاصthe reaction solution was extracted with dichloromethane and 3 times
5. 5
   غسيلwashed with distilled water
6. 6
   أخرىAfter solvent removal
7. 7
   workup.ADDITION)-containing vessel
8. 8
   غسيلwashed
9. 9
   ترشيحfiltered
10. 10
    أخرىdried

الإجراء التجريبي

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%).

المصدر