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Trinuclear rare earth complex based on schiff base ligand as well as solvent thermal preparation method and application of trinuclear rare earth complex

A technology of rare earth complexes and Schiff bases, which can be applied to compounds containing elements of group 3/13 of the periodic table, organic compounds of group 3/13 without C-metal bonds, pharmaceutical formulations, etc., and can solve complex synthesis methods Complicated, difficult complex structures, difficult to purify, etc., to achieve the effect of convenient purification, rapid acquisition, and simple operation

Active Publication Date: 2017-12-22
BENGBU MEDICAL COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, most of the current studies are on the coordination of Schiff bases and transition metal ions. The yields of complexes formed by Schiff bases and rare earth metal ions are generally low, and the synthesis methods of the complexes are complicated, and the known Schiff bases Most of the complexes formed by the alkali and rare earth metal ions are mononuclear or dinuclear complexes, and due to the low yield, it is difficult to purify, which makes it difficult to analyze the structure of the complexes in detail.

Method used

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  • Trinuclear rare earth complex based on schiff base ligand as well as solvent thermal preparation method and application of trinuclear rare earth complex
  • Trinuclear rare earth complex based on schiff base ligand as well as solvent thermal preparation method and application of trinuclear rare earth complex
  • Trinuclear rare earth complex based on schiff base ligand as well as solvent thermal preparation method and application of trinuclear rare earth complex

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Example 1 Preparation of Schiff base ligand:

[0020] Add 4-aminoantipyrine (0.4064 g, 2 mmol) and 40 ml of absolute ethanol into a reactor equipped with a stirrer and a temperature control device, control the temperature at 60-80°C and stir to dissolve, slowly add 2, 3-Dihydroxybenzaldehyde (0.2762 g, 2mmol), keep the reaction mixed evenly, continue to stir for more than 2 hours, control the temperature at 60-80°C, filter and wash the reaction precipitate with absolute ethanol to obtain light brown 2,3-dihydroxy Benzaldehyde acetipyridine, yield 88%.

[0021]

Embodiment 2

[0022] Example 2 Preparation of Trinuclear Rare Earth Complexes Based on Schiff Base Ligands

[0023] Put 0.06 g of 2,3-dihydroxybenzaldehyde antipyridine, 30 mL of absolute ethanol, 15 mL of ethyl acetate, 0.5 mL of triethylamine and 0.08 g of neodymium nitrate hexahydrate into a reaction flask, and put the above The solution was stirred to fully dissolve. Put the solution into a 50 mL reactor liner with a filling degree of 80%, conduct a solvothermal reaction at 60-90°C for 48-36 hours, and then naturally cool to room temperature to obtain a reddish-brown powder crystal. After solid-liquid separation, wash with absolute ethanol for 5 times to obtain 2,3-dihydroxybenzaldehyde antipyridine rare earth neodymium complex crystal.

[0024]

[0025] The crystal structure of 2,3-dihydroxybenzaldehyde antipyridine rare earth neodymium complex is as follows figure 1 Its crystallographic data are shown in Table 1.

[0026] Table 1 Crystallographic data of rare earth neodymium com...

Embodiment 3

[0028] Example 3 Antibacterial Performance Test and Evaluation of Trinuclear Rare Earth Complexes Based on Schiff Base Ligands:

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Abstract

The invention provides a trinuclear rare earth complex based on a schiff base ligand as well as a solvent thermal preparation method and application of the trinuclear rare earth complex. Schiff base formed by 4-aminoantipyrine and aromatic aldehyde with one hydroxyl group respectively at an ortho-position and a meta-position is taken as the ligand; the schiff base ligand is enabled to react with rare earth metal ions for 48-72h in a closed way under the conditions of low temperature and a mixed organic solvent, and is then subjected to coordination in a closed high pressure environment, so that the trinuclear rare earth complex which is clear in structure and stable in properties can be formed; from the view of the structure of the complex, the two hydroxyl oxygen adjacent atoms, which are respectively positioned at the ortho-position and the meta-position of the aromatic aldehyde, not only participate in the coordination, but also form an oxygen bridge so as to link three rare earth metal ions, so that the stability of the complex is improved. The solvent thermal preparation method of the trinuclear rare earth complex is simple and easy to control and convenient in purification, can be used for rapidly obtaining complex crystal, and facilitates structural analysis and performance study; furthermore, antibacterial experiments prove that the trinuclear rare earth complex based on the schiff base ligand has candida species resistance, thus being applied to inhibition of candida species as a bacteriostatic agent.

Description

technical field [0001] The invention relates to the field of metal complexes, in particular to a trinuclear rare earth complex based on a Schiff base ligand and a solvothermal preparation method and application thereof. Background technique [0002] 4-Aminoantipyridine is a widely used pharmaceutical intermediate. 4-Aminoantipyridine derivatives have good antibacterial and antitumor activities, so the synthesis and research of 4-aminoantipyridine derivatives It has always been a research hotspot for scientists. Schiff base mainly refers to a class of organic compounds containing imine or methylimine characteristic group (-RC=N-), which is usually formed by condensation of ammonia and active carbonyl, and has unique biological activity. 4-Aminoantipyridine has good biological properties and coordination properties, and can react with some aromatic aldehydes to form Schiff bases with C=N double bonds by condensation of aldehydes and ammonia. Such Schiff base ligands have pote...

Claims

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Application Information

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IPC IPC(8): C07F5/00A61K31/555A61P31/10
CPCC07B2200/13C07F5/003
Inventor 李文戈陈艳庄毅张敏周鲁宁吴胜顺吴迪刘从森
Owner BENGBU MEDICAL COLLEGE
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