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3,6-diphenyl-9-{9,9'-spirobi[fluorene]-5-yl}-9H-carbazole[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
66%
With rubidium carbonate; tri-tert-butyl phosphine; palladium diacetate; In 5,5-dimethyl-1,3-cyclohexadiene; for 24h;Reflux;
4-bromo-spiro-9,9'-spirobifluorene , <strong>[56525-79-2]3,6-diphenyl-9-H-carbazole</strong> and 29. 2g Rb2CO3 suspended in 250mL of xylene. To the suspension to provide 0. 95g (4. 2mmol) Pd(OAc) 2 and 12. 6ml 1M The butylphosphine solution. The mixture was stirred under reflux for 24 hours. After cooling, the organic phase was separated,150mL of water three times, and then concentrated to dryness in vacuo. The residue was extracted with hot toluene, recrystallized three times from toluene,Then sublimation under high vacuum. The yield was 19. 6g (30. 9mmol), corresponding to 66percent of the theoretical value. Purity according to HPLCIt was 99.9percent.
66%
With rubidium carbonate; tri-tert-butyl phosphine; palladium diacetate; In para-xylene; for 24h;Reflux;
19.2 g (47 mmol) 4-Brom-9-spirobifluorene, 15 g (47 mmol) 3,6-Diphenyl-9-H-carbazole and 29.2 g Rb2CO3 are suspended in 250 mL p-Xylol. To the suspension are given 0.95 g (4.2 mmol) Pd(OAc)2 and 12.6 ml of a 1M solution of Tri-tert-butylphosphine. The mixture is stirred 24 h under reflux. After cooling the organic phase is separated, washed three times with 150 mL water and is subsequently concentrated to dryness in vacuo. The residue is hot extracted with toluene, recrystallized three times from toluene and subsequently sublimated at high vacuum. Yield is 19.6 g (30.9 mmol) corresponding to 66percent of theory. Purity is according to HPLC 99.9percent.
With tri-tert-butyl phosphine; bis(dibenzylideneacetone)-palladium(0); sodium t-butanolate; In toluene; for 12h;Inert atmosphere; Reflux;
The compound 4-bromo-9.9-spirobifluorene (11.94g, 30mmol) and 3,9-bicarbazole (9.99g, 30mmol) were added to a three-necked flask, stirred and dissolved with 300 mL of toluene, protected with nitrogen, and then added. Pd (dba) 2 862.5 mg, 1.5 mmol) and sodium tert-butoxide (5.76 g, 60 mmol), followed by 10 mL of a 10% solution of tri-tert-butylphosphine in toluene. The reaction solution was stirred and refluxed for 12 hours, cooled, and the reaction mixture was washed three times with 100 ml of water.Dry over anhydrous sodium sulfate and then remove the solvent by evaporation.The residue was purified by hydrazine/PE (1:10) through a column.The white solid was obtained as Compound 4 (9.30 g, yield 48%).
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