تفاعل #7290

معادلة التفاعل

fluorene

N-bromosuccinimide

→

desired product

المردود 68.0%

bromo fluorene

المردود 68.0%

المذيبات

propylene carbonate

ظروف التفاعل

المعالجة

1. 1
   أخرىequipped with a stirrer
2. 2
   workup.DISSOLUTIONto make completely dissolved
3. 3
   درجة الحرارةThe reaction mixture was cooled down to room temperature
4. 4
   أخرىto precipitate white solid
5. 5
   ترشيحThe solid was filtered
6. 6
   غسيلthoroughly washed with methanol
7. 7
   أخرىdried
8. 8
   أخرىrecrystallized from ethanol
9. 9
   أخرىto obtain white crystal, which
10. 10
    ترشيحwas filtered
11. 11
    أخرىsufficiently dried in a vacuum oven at 40° C.

الإجراء التجريبي

1.2 litters of propylene carbonate and 160 g (0.96 mol) of fluorene were put into a 2 litter 3-neck round-bottom flask equipped with a stirrer, a thermometer and a reflux condenser under an argon atmosphere, and the resulting mixture was heated to 80° C. so as to make completely dissolved. 179.9 g (1.01 mol) of N-bromosuccinimide was added portionwise to the reaction mixture, and the resultant was stirred at 80° C. for 10 hours. The reaction mixture was cooled down to room temperature to precipitate white solid. The solid was filtered, thoroughly washed with methanol, dried and then recrystallized from ethanol, to obtain white crystal, which was filtered and then sufficiently dried in a vacuum oven at 40° C. to give 160 g (yield: 60%) of the desired product, and its melting point was 102° C.–103° C.

المصدر