Preparation method for crystal of Schiff base vanadyl complex with biological activity

A Schiff base vanadyl and biological activity technology, which is applied in the preparation of imino compounds, compounds of Group 5/15 elements of the periodic table, drug combinations, etc. and other problems, to achieve the effect of good anti-diabetic activity, simple method and easy operation

Inactive Publication Date: 2014-03-19
EAST CHINA NORMAL UNIVERSITY
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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, low bioavailability, and large dosage, so its absorption and utilization rate in organis

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] In the first step, dissolve 0.6532g of 3-chloropropylamine hydrochloride in 25ml of absolute ethanol solvent, add 0.53ml of salicylaldehyde, stir until dissolved, then add 1ml of 5mol / L NaOH aqueous solution to the system, and reflux at 70°C for 3.5 After 1 hour, 10 ml of methanol and 20 ml of chloroform were added to the system to obtain a yellow cloudy mixture.

[0016] The second step is to filter the yellow turbid mixture obtained in the first step, add 10ml of methanol solution containing 0.6624g of vanadyl acetylacetonate to the filtrate, stir and reflux at 55°C for 3 hours and then filter, the filtrate is placed at room temperature for 8 days to precipitate yellow Green crystals.

[0017] The third step is to take out the crystals in the reaction vessel, wash them with methanol three times, then wash them with absolute ethanol and ether three times, place them in a desiccator, and obtain dry and pure crystals after 1 hour, that is, biologically active Schiff base...

Embodiment 2

[0020] In the first step, dissolve 0.6530 g of 3-chloropropylamine hydrochloride solid in 25 ml of anhydrous methanol solvent, add 0.5 ml of salicylaldehyde liquid, stir until dissolved, then add 1 ml of 5 mol / L NaOH aqueous solution to the system, 65 After reflux reaction at °C for 4 hours, 10 ml of methanol and 20 ml of chloroform were added to the system to obtain a yellow turbid mixture.

[0021] The second step is to filter the yellow clear and transparent solution obtained in the first step, add 10ml of methanol solution containing 0.6665g of vanadyl acetylacetonate to the filtrate, stir and reflux at 60°C for 3 hours and then filter, and the filtrate is placed at room temperature for 9 days to precipitate Yellow-green crystals.

[0022] The third step is to take out the crystals at the bottom of the container, wash them with methanol three times, then wash them with absolute ethanol and ether three times respectively, place them in a desiccator, and obtain dry and pure ...

Embodiment 3

[0025] In the first step, dissolve 0.6553g of 3-chloropropylamine hydrochloride solid in 25ml of anhydrous methanol solvent, add 0.54ml of salicylaldehyde liquid, stir until dissolved, then add 1ml of 5mol / L NaOH aqueous solution to the system, 65 After reflux reaction at °C for 4 hours, 10 ml of methanol and 20 ml of chloroform were added to the system to obtain a yellow turbid mixture.

[0026] The second step is to filter the yellow turbid mixture obtained in the first step, add 10ml of methanol solution containing 0.6674g of vanadyl acetylacetonate to the filtrate, stir and reflux at 58°C for 3 hours, then filter, and leave the filtrate at room temperature for 7 days to precipitate yellow Green rhombohedral crystals.

[0027] The third step is to take out the crystals in the reaction vessel, wash them with methanol three times, then wash them with absolute ethanol and ether three times, place them in a desiccator, and obtain dry and pure crystals after 1 hour, that is, bio...

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PUM

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Abstract

The invention discloses a preparation method for a crystal of a Schiff base vanadyl complex with biological activity. The preparation method comprises: taking vanadyl acetylacetonate as a vanadium source, taking a Schiff base obtained through one-step reaction of 3-chloropropylammonium chloride solid and salicylaldehyde as a ligand, standing at room temperature to grow the crystal. Test results show that the crystal shows biological activity and has an inhibition rate on PTP1B enzyme of 46.12-49.29%. By employing one-step synthesis and utilizing a mixed solvent and a room-temperature standing process, the complex crystal with extremely good crystal form can be obtained; the method is simple, easy to operate and short in consumed time; and the synthesized crystal has better anti-diabetes activity compared with same kinds of compounds.

Description

technical field [0001] The invention relates to a method for preparing crystals by using a mixed solvent method, in particular to a method for preparing Schiff base vanadyl complex crystals with biological activity. Background technique [0002] Vanadium is an essential trace element in some animals and plays a very important potential role in the metabolism of glucose. Studies have found that some complexes of inorganic vanadate and vanadium organic ligands have good insulin-like activity, and a few vanadium compounds have been put into clinical trials. Inorganic vanadate has high toxicity, low fat solubility, low bioavailability, and large dosage, so its absorption and utilization rate in organisms is low, and a large amount of use has great toxic and side effects, thus affecting its use in medicine. wide range of applications in the field. In view of this, it is very important to increase the bioavailability of vanadium compounds and reduce their toxicity. A common meth...

Claims

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Application Information

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IPC IPC(8): C07F9/00C07C251/24C07C249/02A61P3/10
Inventor 张其颖李秀彩
Owner EAST CHINA NORMAL UNIVERSITY
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