Reaktion #7290

Reaktionsgleichung

fluorene

N-bromosuccinimide

→

desired product

Ausbeute 68.0%

bromo fluorene

Ausbeute 68.0%

Lösungsmittel

propylene carbonate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeequipped with a stirrer
2. 2
   workup.DISSOLUTIONto make completely dissolved
3. 3
   TemperaturThe reaction mixture was cooled down to room temperature
4. 4
   Sonstigeto precipitate white solid
5. 5
   FiltrationThe solid was filtered
6. 6
   Waschenthoroughly washed with methanol
7. 7
   Sonstigedried
8. 8
   Sonstigerecrystallized from ethanol
9. 9
   Sonstigeto obtain white crystal, which
10. 10
    Filtrationwas filtered
11. 11
    Sonstigesufficiently dried in a vacuum oven at 40° C.

Vorschrift

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.

Quelle