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Preparation method of 2,6-diaminopyridine condensed 3-carboxybenzaldehyde bis-schiff base cobalt complex

A technology of formaldehyde bis-Schiff base cobalt and formaldehyde bis-Schiff base is applied in the field of preparation of 2,6-diaminopyridine condensed 3-carboxybenzaldehyde bis-Schiff base cobalt complex, and can solve the problem of side reactions, unfavorable Product purification and characterization, etc., to achieve the effect of good repeatability, easy popularization and application, and high yield

Active Publication Date: 2017-12-26
GUILIN UNIVERSITY OF TECHNOLOGY
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Problems solved by technology

The advantages of this method are fast reaction, high yield, and convenient and simple operation; the disadvantage is that side reactions occur, which is not conducive to the purification and characterization of the product.

Method used

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  • Preparation method of 2,6-diaminopyridine condensed 3-carboxybenzaldehyde bis-schiff base cobalt complex
  • Preparation method of 2,6-diaminopyridine condensed 3-carboxybenzaldehyde bis-schiff base cobalt complex

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Embodiment

[0024] The present invention is further illustrated below in conjunction with specific examples, but the examples do not limit the protection scope of the present invention.

[0025] (1) Weigh 0.6000 g (4 mmol) of 3-carboxybenzaldehyde and dissolve it in 10 mL of absolute ethanol, and stir evenly with a magnetic force to obtain a colorless, transparent and clear solution.

[0026] (2) Dissolve 0.2180 g (2 mmol) of 2,6-diaminopyridine in 5 mL of absolute ethanol, then slowly drop the colorless, transparent and clear solution prepared in step (1), under nitrogen protection, at 65°C The reaction was carried out under reflux for 4 hours, and a precipitate was formed. After standing, cooling, and suction filtration, a precipitate was obtained.

[0027] (3) The precipitate obtained in step (2) was purified successively by beating method and recrystallization method, and after vacuum drying, a light yellow powder was obtained, which was 2,6-diaminopyridine 3-carboxybenzaldehyde bis ...

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Abstract

The invention discloses a preparation method of a 2,6-diaminopyridine condensed 3-carboxybenzaldehyde bis-schiff base cobalt complex. The preparation method takes 2,6-diaminopyridine and 3-carboxybenzaldehyde as raw materials and absolute ethyl alcohol as a solvent to prepare 2,6-diaminopyridine condensed 3-carboxybenzaldehyde bis-schiff base, without the need of adding a catalyst; the 2,6-diaminopyridine condensed 3-carboxybenzaldehyde bis-schiff base is used as a ligand and reacts with cobalt acetate in an alkaline water solution to prepare the 2,6-diaminopyridine condensed 3-carboxybenzaldehyde bis-schiff base cobalt complex. According to the method disclosed by the invention, the catalyst does not need to be added; the method has the advantages of simple technology, good repeatability and high yield and is convenient for popularization and application.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of 2,6-diaminopyridine 3-carboxybenzaldehyde bis-Schiff base cobalt complex. Background technique [0002] Schiff base is a kind of compound with imino (-C=N-) or imino (-RC=N-) structure formed by the condensation reaction of active amine compounds and carbonyl compounds. The N atom in the C=N bond of this type of compound contains a lone pair of electrons, so this type of compound has good coordination activity. There are many types of Schiff bases, and the synthesis method is simple. Researchers can flexibly choose amines and carbonyl-containing aldehydes or ketones to react to obtain Schiff bases. Various metal elements form metal complexes. [0003] The synthesis of Schiff base is a reaction involving nucleophilic addition, that is, through addition, elimination, rearrangement and other reactions of amine compounds as nucleophiles...

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Application Information

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IPC IPC(8): C07F15/06C07D213/74
CPCC07D213/74C07F15/065
Inventor 刘峥李海莹韩佳星廖秋梅
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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