Metallic copper complex of bipyridine dicarboxylic acid derivatives and preparation method thereof
A technology of bipyridinedicarboxylic acid and complexes, applied in copper organic compounds, 1/11 group organic compounds without C-metal bonds, organic chemical methods, etc., can solve rare, organic and metal-organic complexes. Issues such as few reports and restrictions on the development of ferroelectric materials have achieved the effects of sufficient sources, easy expansion of production, and high purity
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[0024] A typical embodiment of the present invention provides a method for preparing a metal copper complex of bipyridyl dicarboxylic acid derivatives, comprising the following steps:
[0025] 1) Dissolve the ligand dichloride 1,1'-bis(3-benzoic acid)-4,4'-bipyridine in distilled water, then add the template agent 2,2'-biimidazole, and adjust the pH to 1 with HCl ~4, then add CuCl dropwise 2 2H 2 Aqueous solution of O, the ligand, template agent 2,2’-biimidazole and CuCl 2 2H 2 The mol ratio of O is 1: 1: 5~15;
[0026] 2) React at room temperature for 5 to 8 hours, filter, place the filtrate at room temperature, and filter to obtain the metal copper complex of bipyridine dicarboxylic acid derivatives.
[0027] The effect of template agent 2,2'-biimidazole can be analogous to catalyst, does not participate in reaction, plays structure guiding effect, if do not add template agent, will not be able to obtain complex among the present invention; It is well dissolved and HCl ...
Embodiment 1
[0033] Dissolve 0.5 mmol dichloro-1,1’-bis(3-benzoic acid)-4,4’-bipyridine and 0.5 mmol 2,2’-biimidazole in 20 mL H 2 In O, adjust the pH to 3 with 1mol / L HCl, then add 5 mmol CuCl 2 2H 2O is added to it, that is, the molar ratio between the ligand, the template agent, and the metal salt is 1: 1: 10, stirred at room temperature for 5 hours, filtered to obtain a blue filtrate, left to evaporate at 25°C, and a blue color will appear after 3 weeks Crystals were collected by filtration in a 35% yield.
[0034] Structure determination of the complex:
[0035] The crystal sample obtained in Example 1 was fixed on a Bruker SMART 1000 CCD surface probe diffractometer, and the graphite monochromator MoKα was used as the radiation source to collect the X-Ray diffraction data of the sample pair with a wavelength of 0.71073 Å. In the ω-scan mode, the diffraction data were corrected for LP factors and empirical absorption. After restoring all X-Ray diffraction patterns to diffraction...
Embodiment 2
[0043] Dissolve 0.5 mmol dichloro-1,1’-bis(3-benzoic acid)-4,4’-bipyridine and 0.5 mmol 2,2’-biimidazole in 20 mL H 2 In O, adjust the pH to 1 with 1mol / L HCl, then add 5 mmol CuCl 2 2H 2 O is added to it, that is, the molar ratio between the ligand, the template agent, and the metal salt is 1: 1: 15, stirred at room temperature for 5 hours, filtered to obtain a blue filtrate, left to evaporate at 25°C, and a blue color will appear after 3 weeks Crystals were collected by filtration in a 25% yield.
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