Fluorene → 1-Bromo-9h-fluorene

温度

80 °C

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.

1. customequipped with a stirrer
2. dissolutionto make completely dissolved
3. temperatureThe reaction mixture was cooled down to room temperature
4. customto precipitate white solid
5. filtrationThe solid was filtered
6. washthoroughly washed with methanol
7. customdried
8. customrecrystallized from ethanol
9. customto obtain white crystal, which
10. filtrationwas filtered
11. customsufficiently dried in a vacuum oven at 40° C.

ORDレコード

ord-a37453ac498b403e8ea58f83bd8e7af0

出典データセット

uspto-grants-2006_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07084231B2