Sulfur-sulfur bond containing dipolymacrocyclic nickel (II) complex and in-situ synthesis method thereof

A technology of in-situ synthesis and complexes, which is used in pharmaceutical formulations, medical preparations with inactive ingredients, drug combinations, etc., to achieve the effect of wide application prospects

Inactive Publication Date: 2019-06-21
GUANGXI NORMAL UNIV
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  • 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 dimeric macromolecules containing sulfur-sulfur bonds. A Report of Cyclic Ligands Forming Ni(Ⅱ) Complexes

Method used

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  • Sulfur-sulfur bond containing dipolymacrocyclic nickel (II) complex and in-situ synthesis method thereof
  • Sulfur-sulfur bond containing dipolymacrocyclic nickel (II) complex and in-situ synthesis method thereof
  • Sulfur-sulfur bond containing dipolymacrocyclic nickel (II) complex and in-situ synthesis method thereof

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Embodiment

[0016] A method for in-situ synthesis of dimeric macrocyclic nickel (II) complexes 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 0.0475g nickel dichloride hexahydrate NiCl 2 ·6H 2 O, then added to 4mL methanol and 6mL 1,4-dioxane, and the mixture was stirred and reacted at room temperature for 6h;

[0018] (2) Filter the above mixed solution, put the filtrate in a beaker, and let it volatilize naturally at room temperature to obtain single crystal grade purple flaky crystals.

[0019] see figure 1 , Example Schematic diagram of the molecular structure of dimeric macrocyclic nickel (II) complexes containing sulfur-sulfur bonds. For the convenience of observation, the two external chloride ions are deleted. It can be clearly seen from the figure that the inner boundary of the complex is composed of a Ni 2+ , a macrocyclic ligand (H 4 L 1 ) and two H 2 O molecular composition, Ni 2+ io...

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Abstract

The invention discloses a sulfur-sulfur bond containing dipolymacrocyclic nickel (II) complex and an in-situ synthesis method thereof. The nickel complex has a chemical formula [Ni(H4L1)(H2O)2]*2Cl, in the formula, H4L1 is a macrocyclic ligand formed by two 3,3'-di(5-sulfydryl-1,2,4-triazole) through sulfur-sulfur bonds. The in-situ synthesis method of the nickel (II) complex comprises the following steps: (1) weighing 0.04-0.05g of 3,3'-di(5-sulfydryl-1,2,4-triazole) and 0.04-0.05g of hexahydrate nickel dichloride NiCl2*6H2O, adding 3-5mL of methanol and 5-7mL of 1,4-dioxane, and stirring toenable the mixed liquid to react for 6-7 hours at the room temperature; (2) filtering the mixed liquid, putting filtrate into a flask, and naturally volatizing the filtrate at the room temperature, thereby obtaining a single crystal grade purple flaky crystal. The nickel (II) complex has potential application values in antibacterial, anti-tumor and medicine targeted release carriers, and the like,and the method has great application prospects in in-situ synthesis of sulfur-sulfur bond containing macrocyclic metallic complexes.

Description

technical field [0001] The invention relates to a nickel complex, in particular to a dimeric macrocyclic nickel (II) complex containing a sulfur-sulfur bond 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 dimeric macromolecules containing sulfur-sulfur bonds. A report on ring ligands and further formation of Ni(II) complexes. [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 , 2,4-triazole) i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D513/22A61K47/22A61K47/54A61P35/00A61P31/04A61P31/10
Inventor 蒋毅民王慧许小陵
Owner GUANGXI NORMAL UNIV
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