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Tetrameric macrocyclic trinuclear iron complex containing sulfur-sulfur bonds and in-situ synthesis method thereof

An iron complex, in-situ synthesis technology, applied in organic chemical methods, drug combinations, topical antibacterial agents, etc., to achieve the effect of wide application prospects

Inactive Publication Date: 2019-07-05
GUANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although there are many literature reports on in situ reactions, no 3,3'-bis(5-mercapto-1,2,4-triazole) is oxidized to form tetrameric macromolecules containing sulfur-sulfur bonds. Cyclic Ligands and Formation of Trinuclear Iron Complexes Report

Method used

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  • Tetrameric macrocyclic trinuclear iron complex containing sulfur-sulfur bonds and in-situ synthesis method thereof
  • Tetrameric macrocyclic trinuclear iron complex containing sulfur-sulfur bonds and in-situ synthesis method thereof
  • Tetrameric macrocyclic trinuclear iron complex containing sulfur-sulfur bonds and in-situ synthesis method thereof

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Embodiment

[0016] A method for in-situ synthesis of a tetrameric macrocyclic trinuclear iron complex containing sulfur-sulfur bonds, comprising the steps of:

[0017] (1) Weigh 0.0400g 3,3’-bis(5-mercapto-1,2,4-triazole) (H 4 L) and 0.0808g iron nitrate nonahydrate Fe(NO 3 ) 3 9H 2 O, mixed in 8 mL dimethylformamide (DMF), and the mixture was stirred and reacted at room temperature for 6 h;

[0018] (2) The above mixture was filtered, and the filtrate was placed in a 50 mL beaker, and naturally volatilized at room temperature to obtain single crystal grade black flaky crystals.

[0019] see figure 1 , a schematic diagram of the molecular structure of the four polycyclic macrocyclic trinuclear iron complexes containing sulfur-sulfur bonds in the embodiment. It can be seen clearly from the figure that the complex is a trinuclear iron structure composed of three iron ions [2 Fe ( Ⅲ) and one Fe (II)], one macrocyclic ligand and five waters. Among them, Fe1 coordinates with the four N ...

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Abstract

The invention discloses a tetrameric macrocyclic trinuclear iron complex containing sulfur-sulfur bonds and an in-situ synthesis method thereof. A chemical formula of the iron complex is [Fe3(L1) 5H2O], wherein H8L1 is a macrocyclic ligand formed by four 3,3'-di(5-mercapto-1,2,4-triazole) through sulfur-sulfur bonds. The in-situ synthesis method of the iron complex comprises the following steps: (1) weighing 0.04-0.05 g of 3,3'-di(5-mercapto-1,2,4-triazole) and 0.08-0.09 g of ferric nitrate nonahydrate Fe(NO3)3 9H2O, mixing them in a 8-9 mL dimethylformamide and enabling the mixed solution tobe subjected to stirring reacction at room temperature for 6-7 hours; (2) filtering the mixed solution, placing the filtrate in a beaker, and executing natural volatilization at room temperature to obtain single-crystal-grade black flaky crystals. The iron complex has a potential application value on the aspects of bacterium and tumor resistance, targeted release as a carrier and the like, and themethod has the wide application prospect on the aspect of in-situ synthesis of macrocyclic metal complexes containing sulfur-sulfur bonds.

Description

technical field [0001] The invention relates to an iron complex, in particular to a sulfur-sulfur bond-containing tetramerized macrocyclic trinuclear iron complex and an in-situ synthesis method thereof. Background technique [0002] In situ reaction is one of the hotspots in coordination chemistry research. Although there are many literature reports on in situ reactions, no 3,3'-bis(5-mercapto-1,2,4-triazole) is oxidized to form tetrameric macromolecules containing sulfur-sulfur bonds. A report on the formation of trinuclear iron complexes by ring ligands. [0003] Sulfur-containing triazoles are widely used as intermediates in medicine, pesticides and other fields, and their complexes with metal ions also have good antibacterial and anticancer activities. When a compound containing a sulfur-sulfur bond reaches a tumor cell, a sulfur-sulfur bond breaking reaction will occur due to glutathione present in a large amount in the cell, therefore, by 3,3'-bis(5-mercapto-1 , 2,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D513/22A61P31/00A61P31/04A61P31/02A61P35/00
CPCA61P31/00A61P31/02A61P31/04A61P35/00C07B2200/13C07D513/22
Inventor 蒋毅民王慧许小陵
Owner GUANGXI NORMAL UNIV
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