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Preparation method for Schiff base oxovanadium complex crystal with bioactivity

A Schiff base vanadyl and biologically active technology, which is applied in the field of preparation of Schiff base vanadyl complex crystals, can solve the problems of high toxicity, low bioavailability, and wide application of inorganic vanadates, and achieve good resistance Diabetic activity, simple method, and short-term effect

Inactive Publication Date: 2015-09-30
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Inorganic vanadate has high toxicity, low fat solubility and low bioavailability, thus affecting its wide application in the field of medicine

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] In the first step, dissolve 0.4498g of alanine in 10ml of water, stir in a three-neck flask until completely dissolved, dissolve 1.3288g of vanadyl acetylacetonate in a mixed solvent of 10ml of chloroform and 10ml of anhydrous methanol, and dissolve it completely Transfer to a three-necked bottle filled with glycine aqueous solution, and heat under reflux at 60°C for 3 hours to obtain a blue-green solution.

[0016] Step 2 Add 15ml of anhydrous methanol solution dissolved with 0.7835g of 2,2’-bipyridine to the blue-green solution obtained in Step 1, stir and reflux at 60°C for 3 hours, then stop the reaction. After cooling, filter, move the filtrate to a 25ml beaker, and place it in a refrigerator at 0°C to 4°C for 3 to 5 days to precipitate yellow-brown diamond-shaped crystals.

[0017] The third step is to take out the crystals in the reaction vessel, wash them three times with anhydrous methanol, then wash them three times with absolute ethanol and ether, and place t...

Embodiment 2

[0020] In the first step, dissolve 0.4463g of alanine in 10ml of water, stir in a three-neck flask until completely dissolved, dissolve 1.3268g of vanadyl acetylacetonate in a mixed solvent of 10ml of chloroform and 10ml of anhydrous methanol, and dissolve it completely Transfer to a three-necked bottle filled with glycine aqueous solution, and heat under reflux at 60°C for 3 hours to obtain a blue-green solution.

[0021] Step 2 Add 15ml of anhydrous methanol solution dissolved with 0.7863g of 2,2’-bipyridine to the blue-green solution obtained in Step 1, stir and reflux at 60°C for 3 hours, then stop the reaction. After cooling, filter, move the filtrate to a 25ml beaker, and place it in a refrigerator at 0°C to 4°C for 3 to 5 days to precipitate yellow-brown diamond-shaped crystals.

[0022] The third step is to take out the crystal in the reaction vessel, wash it three times with anhydrous methanol first, then wash it three times with absolute ethanol and diethyl ether, pl...

Embodiment 3

[0025] In the first step, dissolve 0.4412g of alanine in 10ml of water, stir in a three-neck flask until completely dissolved, dissolve 1.3256g of vanadyl acetylacetonate in a mixed solvent of 10ml of chloroform and 10ml of anhydrous methanol, and dissolve it completely Transfer to a three-necked bottle filled with glycine aqueous solution, and heat under reflux at 60°C for 3 hours to obtain a blue-green solution.

[0026] Step 2 Add 15ml of anhydrous methanol solution dissolved with 0.7863g of 2,2’-bipyridine to the blue-green solution obtained in Step 1, stir and reflux at 60°C for 3 hours, then stop the reaction. After cooling, filter, move the filtrate to a 25ml beaker, and place it in a refrigerator at 0°C to 4°C for 3 to 5 days to precipitate yellow-brown diamond-shaped crystals.

[0027] The third step is to take out the crystal in the reaction vessel, wash it three times with anhydrous methanol first, then wash it three times with absolute ethanol and diethyl ether, pl...

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Abstract

The invention discloses a preparation method for a Schiff base oxovanadium complex crystal with bioactivity. In the method, vanadyl acetylacetonate is used as a vanadium source, Schiff base obtained through one-step reaction of acetylacetone in the vanadyl acetylacetonate and alanine is used as a ligand, 2, 2-dipyridyl is used as a second ligand; the materials are placed in a refrigerator to enable the crystal to grow; a test result shows that the crystal has bioactivity, the average inhibition ratio to PTP1B enzymes is 70.61-70.69%, and the IC50 is equal to 11.27-11.36 [mu]g / mL (dimethyl sulfoxide is used as a solvent). According to the invention, the complex crystal with a good crystal form and high activity can be obtained through the adoption of one-step synthesis and the utilization of a mixed solvent; the method is simple, easy to operate and short in consumed time; compared with similar compounds, the synthesized crystal has good antidiabetic activity.

Description

technical field [0001] The invention relates to a method for preparing crystals by using a mixed solvent method, specifically, a method for preparing Schiff base vanadyl complex crystals with biological activity. Background technique [0002] Vanadium is an essential trace element in humans and animals, and plays a very important potential role in the metabolism of glucose. Protein tyrosine phosphatase (PTP1B) is involved in the physiological processes of various organisms and is closely related to insulin sensitivity. The researchers regard PTP1B enzyme as a new target for diabetes treatment. 50 When the value (the concentration of vanadium preparation when the inhibition rate reaches 50%) is low, any substance with a high inhibition rate on PTP1B enzyme can promote the transduction of insulin signal, and may become a potential new drug for treating diabetes . Studies have found that some complexes of inorganic vanadate and vanadium organic ligands have special insulin-li...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/00A61P3/10
Inventor 张其颖殷宁李秀彩
Owner EAST CHINA NORMAL UNIV
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