反应详情

温度

130 °C

In a 200 ml-three-necked flask, 6.00 g (20.5 mM) of 2-octanoylfluorene, 3.06 ml (50.4 mM) of hydrazine hydrate (80% aqueous solution), 4.20 g (63.6 mM) of potassium hydroxide and 60 ml of diethyleneglycol were placed, followed by heating to about 130° C. to dissolve the mixture. Then, the mixture was gradually heated to 210°-217° C., followed by stirring for 3 hours and 40 minutes under heating. After the reaction, the reaction mixture was cooled and poured into 250 ml of water to precipitate a crystal. The crystal was recovered by filtration and dissolved in toluene, followed by washing with water, drying with anhydrous sodium sulfate and distilling-off of the solvent. The residue was purified by silica gel column chromatography (eluent: toluene/hexane=1/2) to obtain 4.58 g of 2-octylfluorene.

1. dissolutionto dissolve the mixture
2. temperatureThen, the mixture was gradually heated to 210°-217° C.
3. temperatureunder heating
4. customAfter the reaction
5. temperaturethe reaction mixture was cooled
6. customto precipitate a crystal
7. filtrationThe crystal was recovered by filtration
8. dissolutiondissolved in toluene
9. washby washing with water
10. dry with materialdrying with anhydrous sodium sulfate and distilling-off of the solvent
11. customThe residue was purified by silica gel column chromatography (eluent: toluene/hexane=1/2)