반응 #7290

반응 방정식

fluorene

N-bromosuccinimide

→

desired product

수율 68.0%

bromo fluorene

수율 68.0%

용매

propylene carbonate

반응 조건

후처리

1. 1
   기타equipped with a stirrer
2. 2
   workup.DISSOLUTIONto make completely dissolved
3. 3
   온도The reaction mixture was cooled down to room temperature
4. 4
   기타to precipitate white solid
5. 5
   여과The solid was filtered
6. 6
   세척thoroughly washed with methanol
7. 7
   기타dried
8. 8
   기타recrystallized from ethanol
9. 9
   기타to obtain white crystal, which
10. 10
    여과was filtered
11. 11
    기타sufficiently dried in a vacuum oven at 40° C.

실험 절차

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.

출처