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[ CAS No. 134008-76-7 ] {[proInfo.proName]}

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Chemical Structure| 134008-76-7
Chemical Structure| 134008-76-7
Structure of 134008-76-7 * Storage: {[proInfo.prStorage]}
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Product Details of [ 134008-76-7 ]

CAS No. :134008-76-7 MDL No. :MFCD28975113
Formula : C48H36N2 Boiling Point : -
Linear Structure Formula :- InChI Key :-
M.W : 640.81 Pubchem ID :-
Synonyms :

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Application In Synthesis of [ 134008-76-7 ]

* 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.

  • Downstream synthetic route of [ 134008-76-7 ]

[ 134008-76-7 ] Synthesis Path-Downstream   1~3

  • 2
  • [ 1591-31-7 ]
  • [ 531-91-9 ]
  • [ 98-95-3 ]
  • potassium carbonate [ No CAS ]
  • copper [ No CAS ]
  • [ 134008-76-7 ]
  • 3
  • [ 3001-15-8 ]
  • [ 32228-99-2 ]
  • [ 134008-76-7 ]
YieldReaction ConditionsOperation in experiment
91.47% With 3,5-ditertbutyl salicylic acid; potassium carbonate; sodium hydrogensulfite In 1-dodecylbenzene; xylene at 210℃; for 11h; Inert atmosphere; 1 Example 1Synthesis of a 4,4'-bis{(biphenyl-4-il)-phenylamino}biphenylThe following compounds were put into a reaction vessel purged with nitrogen and were mixed together. (Biphenyl-4-il)-phenylamine 8.50 g (34.6 millimols) 4,4'-Diiodobiphenyl 5.85 g (14.4 millimols) Copper powder 0.09 g (1.44 millimols) 3,5-Di(tert-butyl)-2-hydroxybenzenecarboxylic 0.36 g (1.44 millimols) acid Potassium carbonate 5.97 g (43.2 millimols) Sodium hydrogensulfite 0.45 g (4.32 millimols) Dodecylbenzene 10 ml Xylene 20 ml The above mixture put into the reaction vessel was heated at 210° C. for 11 hours with stirring while distilling off xylene.After the reaction has been finished, the obtained reaction solution was analyzed by the HPLC to confirm the terminating point of the reaction. The HPLC analyzer possessed the following specifications.HPLC analyzer: Model L-7100 manufactured by Hitachi, Ltd. Column: Inertsil ODS-3 manufactured by GL Science Co., 4.6 mm in inner diameter, 250 mm in length, Flow rate: 1.0 ml/min, Column temperature: 40° C., Detection wavelength: 254 nm Eluent: acetonitrile/THF=9/1 (v/v) The results of HPLC analysis at the terminating point of the reaction were as described below in terms of the peak area ratios of the HPLC. 4,4'-Bis{(biphenyl-4-il)-phenylamino}biphenyl (object product): 90.6% 4,4'-Diiodobiphenyl (starting material): 0.64% Monoiodide (intermediate product): 0.75% The above reaction solution was cooled, toluene was added thereto to remove undissolved matters by filtration, and the filtrate was concentrated to obtain a concentrated product thereof.Hexane was added to the concentrated product, precipitated crystals were picked up by filtration, the obtained coarse crystals were refined by crystallization by using a mixed solvent of toluene/hexane to obtain an object 4,4'-bis{(biphenyl-4-il)-phenylamino}biphenyl in powdery form in an amount of 8.46 g (yield, 91.7%).The obtained powder was put to the NMR analysis (1H-NMR) to confirm the structure. A chart of analysis thereof is shown in FIG. 1.
88% With copper; potassium carbonate; sodium thiosulfate In 5,5-dimethyl-1,3-cyclohexadiene at 210℃; for 20h; 1 Synthesis of 4,4'-bis[biphenyl-4-yl(phenyl)amino]biphenyl (Compound 1-1) N-(phenyl)-biphenyl-4-amine (10.0 g), 4,4′-diiodobiphenyl (7.2 g), potassium carbonate (7.4 g), sodium hyposulfite (0.6 g), a copper powder (0.1 g), dodecylbenzene (7.2 mL), and xylene (7.2 mL) were added into a nitrogen-substituted reaction vessel. The mixture was stirred at 210° C. for 20 hours. Toluene was added while cooling the reaction solution, hot filtration was carried out at 50° C., and the filtrate was cooled to room temperature, then methanol was added while stirring, and the precipitated solid was collected by filtration. The obtained solid is recrystallized with toluene-methanol, whereby a yellowish white powder of 4,4′-bis[biphenyl-4-yl(phenyl)amino]biphenyl (Compound 1-1; 10.0 g; yield 88%) was obtained. The structure of the obtained yellowish white powder was identified by NMR. 1H-NMR (CDCl3) detected 36 hydrogen signals, as follows. δ (ppm)=7.38-7.72 (16H), 7.10-7.38 (18H), 7.07-7.08 (2H).
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