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CAS No. : | 1060735-14-9 | MDL No. : | MFCD22581311 |
Formula : | C30H20N2 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | GKTLHQFSIDFAJH-UHFFFAOYSA-N |
M.W : | 408.49 | Pubchem ID : | 59306629 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P273-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H319-H412 | Packing Group: | |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With N2;tris-(dibenzylideneacetone)dipalladium(0); Pd2(dba)3; In tetrahydrofuran; 5,5-dimethyl-1,3-cyclohexadiene; hexane; dichloromethane; toluene; | A mixture of 9-phenyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-9H-carbazole (12 g, 32.5 mmol), 3-bromo-9H-carbazole (6.66 g, 27.1 mmol), and potassium phosphate (34.5 g, 162 mmol) in 500 mL of toluene and 50 mL of H2O was bubbled with N2 for 20 min. Dicyclohexyl(2',6'-dimethoxybiphenyl-2-yl)phosphine (0.445 g, 1.083 mmol) and Pd2(dba)3 (0.248 g, 0.271 mmol) were then added, and the mixture was heated to reflux under N2 for 5 h. TLC indicated the reaction was done. The reaction was extracted with dichloromethane and washed with brine and dried with magnesium sulfate. The solution was heated up to boil. Hexane was added. The dichloromethane was boiled off and hexanes volume reached about 1200 mL. Precipitate formed during boiling off dichloromethane. The solution was cooled to room temperature and stirred overnight. The precipitate was filtered and dissolved in THF and ran a short silica gel plug. After dried under vacuum at 60 C., 9.6 g (87%) of product was obtained. Synthesis of Compound 1. A mixture of <strong>[5408-56-0]2-iododibenzo[b,d]furan</strong> (2.59 g, 8.81 mmol), 9-phenyl-9H,9'H-3,3'-bicarbazole (3 g. 7.34 mmol), and sodium t-butoxide (1.764 g, 18.36 mmol) in 200 mL of xylene was bubbled with N2 for 20 min. Dicyclohexyl(2',6'-dimethoxybiphenyl-2-yl)phosphine (0.121 g, 0.294 mmol) and Pd2(dba)3 (0.067 g, 0.073 mmol) were then added, and the mixture was heated to reflux under N2 for 24 h. The mixture was cooled and filtered through Celite. After solvent evaporation, the residue was coated on Celite and purified by column chromatography 3.7 g of product was obtained after column. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With dicyclohexyl-(2',6'-dimethoxybiphenyl-2-yl)-phosphane; sodium t-butanolate;tris-(dibenzylideneacetone)dipalladium(0); In xylene; for 24h;Inert atmosphere; Reflux; | Compound 1[0130] Synthesis of Compound 1. A mixture of <strong>[5408-56-0]2-iododibenzo[b,d]furan</strong> (2.59 g, 8.81 mmol), 9-phenyl-9H,9'H-3,3'-bicarbazole (3 g, 7.34 mmol), and sodium t-butoxide (1.764 g, 18.36 mmol) in 200 mL of xylene was bubbled with N2 for 20 min. Dicyclohexyl(2',6'- dimethoxybiphenyl-2-yl)phosphine (0.121 g, 0.294 mmol) and Pd2(dba)3 (0.067 g, 0.073 mmol) were then added, and the mixture was heated to reflux under N2 for 24 h. The mixture was cooled and filtered through Celite. After solvent evaporation, the residue was coated on Celite and purified by column chromatography 3.7 g of product was obtained after column. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
65% | With tris-(dibenzylideneacetone)dipalladium(0); sodium t-butanolate; tri tert-butylphosphoniumtetrafluoroborate; In 5,5-dimethyl-1,3-cyclohexadiene; for 8h;Inert atmosphere; Reflux; | [0176] In an argon atmosphere, <strong>[13438-50-1]3-bromofluoranthene</strong> (2.3 g, 8.1 mmol), Intermediate 1-1 (3 g, 7.3 mmol), Pd2(dba)3(0.14 g,0.15 mmol), P(tBu)3HBF4 (0.17 g, 0.6 mmol), sodium t-butoxide (1.1 g, 11 mmol), and dry xylene (30 mL) werecharged in a three-necked flask in this order, and the resultant mixture was refluxed under heating for 8 h.The solid generated by adding water to the reaction liquid was successively washed with hexane and methanol and then purified by silica gel column chromatography, to obtain Compound 1-1 (2.9 g, yield: 65percent). FD-MS analysis: m/e = 608 for molecular weight of 608. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
86% | With dicyclohexyl-(2',6'-dimethoxybiphenyl-2-yl)-phosphane; tris-(dibenzylideneacetone)dipalladium(0); sodium t-butanolate; In 5,5-dimethyl-1,3-cyclohexadiene;Inert atmosphere; Reflux; | 10132] A solution of <strong>[26608-06-0]3-bromodibenzo[b,d]furan</strong> (2.8 g,11.33 mmol), 9-phenyl-9H,9?H-3,3?-bicarbazole (4.63 g,11.33 mmol), Pd2(dba)3 (0.21 g, 0.23 mmol), SPhos (0.13 g,0.32 mmol) and tert-l3uONa (1.63 g, 17.0 mmol) in xylene(150 ml) was refluxed under nitrogen overnight. Uponevaporation of the solvent, the residue was purified bycolunm chromatography on silica gel with heptane/ethylacetate (95/5 to 90/10, v/v) as eluent and recrystallized fromheptane to yield Compound Al (5.6 g, 86%) as a white solid. |