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A kind of o-vanillin bisethylenediamine vanadium complex, its synthesis method and its application

A technology of vanadium bis-ethylenediamine and o-vanillin is applied in pharmaceutical formulations, organic chemical methods, preparation of imino compounds, etc., and can solve problems such as aggravating diabetes, tumors, and cell oxidative damage.

Active Publication Date: 2021-09-21
HENAN UNIV OF CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Under normal circumstances, the scavenging and generation of free radicals in the body maintains a dynamic balance, but excessive free radicals can cause oxidative damage to normal cells in the body, thereby inducing the occurrence of diseases and aging. Oxidative damage can not only lead to or even aggravate Diabetes and tumors and other diseases, so it is of great significance to find active free radical scavengers

Method used

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  • A kind of o-vanillin bisethylenediamine vanadium complex, its synthesis method and its application
  • A kind of o-vanillin bisethylenediamine vanadium complex, its synthesis method and its application
  • A kind of o-vanillin bisethylenediamine vanadium complex, its synthesis method and its application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Example 1 o-vanillin bisethylenediamine vanadium complex (C 18 h 22 N 2 o 7 V) Synthesis

[0036] (1) Disperse 0.02 mmol of the ligand o-vanillin bisethylenediamine in 1 mL of dimethylformamide to prepare o-vanillin bisethylenediamine solution;

[0037] 0.0020mmol VOSO 4 Disperse in 3mL water to prepare VOSO 4 solution;

[0038] (2) Add o-vanillin bisethylenediamine solution dropwise to VOSO 4 In solution, it is prepared into o-vanillin bisethylenediamine and VOSO 4 The mixed solution; among them, o-vanillin bisethylenediamine and VOSO 4 The molar ratio of the substance is 1:1;

[0039] (3) Put the mixed solution of step (2) in a polytetrafluoroethylene-lined stainless steel reactor, react at 80°C for 72h, then cool down to room temperature at a rate of 5°C / h, and dry naturally to obtain a brown-red Blocky crystals, that is, o-vanillin bisethylenediamine vanadium complex.

Embodiment 2

[0040] Example 2 o-vanillin bisethylenediamine vanadium complex (C 18 h 22 N 2 o 7 V) Structural characterization

[0041] 1. Infrared Spectrum

[0042] Adopt Nicolet NEXUS 470-FTIR type infrared spectrometer to carry out infrared spectrum test to the o-vanillin bisethylenediamine vanadium complex that embodiment 1 obtains (using KBr tablet method, scanning under room temperature, test range is 400~4000cm-1 ). Infrared spectrum characteristic absorption peak (cm -1 ): 3410, 2907, 1637, 1600, 1470, 1440, 1243, 1216.

[0043] 2. Single crystal structure analysis

[0044] Adopt Rigaku Saturn 724 CCD diffractometer to carry out crystal structure test to the o-vanillin bisethylenediamine vanadium complex that embodiment 1 obtains, test result is:

[0045] The vanillin bisethylenediamine vanadium complex is a monoclinic crystal system, P2 1 / n point group; unit cell parameters α=90°, β=93.988(3)°, γ=90°; Z=4; Dc=1.508Mg / m 3 ; I>2σ(I), R 1 =0.0455, wR 2 = 0.1119; al...

Embodiment 3

[0048] Example 3 Scavenging effect of o-vanillin bisethylenediamine ligand and its vanadium complex on superoxide anion free radicals

[0049] superoxide anion radical O 2 - It has strong reactivity and short life, so the determination of its activity is not easy to use direct method. Indirect determination of O by pyrogallol autoxidation 2 - clearing effect. Include the following steps:

[0050] (1) Preparation of solution

[0051] Preparation of 0.10mol / L hydrochloric acid solution: accurately pipette 2.25mL of 36.5% concentrated hydrochloric acid into a 250mL volumetric flask, distilled water to volume, and mix well.

[0052] Preparation of 10.0mmol / L hydrochloric acid solution: Accurately pipette 20.0mL of 0.10mol / L hydrochloric acid solution into a 200mL volumetric flask, dilute to volume with double distilled water, and mix well.

[0053] Tris-HCl buffer solution (0.05mol / L Tris, pH=8.20±0.10): Weigh 1.5143g of trishydroxymethylaminomethane, take 57.25mL of 0.10mo...

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Abstract

The invention discloses an o-vanillin bisethylenediamine vanadium complex, a synthesis method and an application thereof. The chemical formula of the o-vanillin bisethylenediamine vanadium complex is: {[VOL·(H 2 O)]·H 2 O} n , the molecular formula is: C 18 h 22 N 2 o 7 V; The ligand of the o-vanillin bisethylenediamine vanadium complex is o-vanillin bisethylenediamine. The present invention uses o-vanillin bisethylenediamine as a ligand, and adopts a hydrothermal method to convert VOSO 4 React with o-vanillin bisethylenediamine to coordinate ligands with metal ions to obtain a new o-vanillin bisethylenediamine vanadium complex. The complex is expected to be applied in the fields of anti-oxidation and anti-cancer. The synthesis method of the invention is simple, convenient and safe, has mild reaction conditions, high yield and high purity, and is beneficial to subsequent tests.

Description

technical field [0001] The invention relates to an o-vanillin bisethylenediamine vanadium complex, a synthesis method and an application thereof, belonging to the field of coordination chemistry. Background technique [0002] Schiffer's base refers to a class of organic compounds containing imine or methimine characteristic groups, which are usually prepared by reacting primary amines with active carbonyl compounds. Due to its relatively easy synthesis, it can flexibly perform selective reactions, and appropriately change the substituent group and its chemical environment, and it is easy to derive a series from chain to ring closure, from monodentate to multidentate, with different properties and multiple structures. Variable Schiff base ligands, such as monodentate Schiff bases, bidentate Schiff bases, asymmetric Schiff bases, and isobis Schiff bases. Under certain conditions, Schiffer's base can form metal complexes with different stability with most metal ions in the per...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C249/02C07C251/24A61K31/137A61P35/00G01N21/31
CPCC07B2200/13C07C249/02C07C251/24G01N21/31
Inventor 刘艳菊崔红新杨怀霞杨艳秋李曼曼李娅雪温东晓石福涛
Owner HENAN UNIV OF CHINESE MEDICINE
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