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2-Pyridineformaldehyde acetal 1,3 diamino-2-propanol Schiff base tetranuclear dysprosium cluster and its synthesis method and application

A technology of pyridine carboxaldehyde and synthesis method, which is applied to the 3/13 group organic compounds without C-metal bonds, the compounds containing the 3/13 group elements of the periodic table, chemical instruments and methods, etc., which can solve the inconvenient modeling calculation. and other problems, to achieve the effect of simple and easy operation, good reproducibility and controllable conditions of the synthesis method.

Inactive Publication Date: 2020-01-31
GUANGXI NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

High-nuclear complexes often have complex and beautiful structures, and there are too many factors affecting the magnetic properties of high-nuclear complexes, which is not convenient for modeling and calculation
However, there has not yet been seen that 2-pyridinecarbaldehyde and 1,3-diamino-2-propanol have undergone in situ reaction to spontaneously assemble to form a ligand and then combine with Dy(ClO 4 ) 3 ·6H 2 Reaction of O to 1,3-diamino-2-propanol Schiff base tetranuclear dysprosium clusters obtained from 2-pyridine formaldehyde

Method used

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  • 2-Pyridineformaldehyde acetal 1,3 diamino-2-propanol Schiff base tetranuclear dysprosium cluster and its synthesis method and application
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  • 2-Pyridineformaldehyde acetal 1,3 diamino-2-propanol Schiff base tetranuclear dysprosium cluster and its synthesis method and application

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1) Weigh 0.2142g (2mmol) of 2-pyridinecarbaldehyde and dissolve it in 5mL of acetonitrile, and dissolve 0.09012g (1mmol) of 1,3-diamino-2-propanol in 5mL of ethanol. The acetonitrile solution of formaldehyde is slowly added to the ethanol solution of 1,3-diamino-2-propanol, and mixed evenly to obtain the aldehyde-amine mixture, which is set aside;

[0025] 2) Weigh the metal salt Dy(ClO 4 ) 3 ·6H 2 Add O (0.1mmol, 56.8mg) into a glass bottle with a volume of about 20mL, use a pipette to draw 1mL of the above-mentioned aldehyde-amine mixture into the glass bottle, and then add 1.5mL of acetonitrile to it, so that the ethanol and amine in the glass bottle The volume ratio of acetonitrile is 1:4 (0.5mL and 2mL respectively), then add 10 μL triethylamine to it, shake well (the pH of the solution at this time=8.1); then seal the glass bottle mouth with aluminum foil, The reaction was allowed to stand at room temperature for 24 hours, taken out, wrapped with cotton wool an...

Embodiment 2

[0062] Repeat Example 1, the difference is:

[0063] 1) After adding 1mL of aldehyde-amine mixture into the glass bottle, add 1mL of acetonitrile to it, so that the volume ratio of ethanol and acetonitrile in the mixed solvent is 1:3;

[0064] 2) adjust the pH of the system to 7.8 with triethylamine;

[0065] 3) The reaction is carried out at 20° C., and the reaction time is 48 hours.

[0066] Colorless crystals with long cut corners were obtained with a yield of 29.3%. The resulting product was characterized for its structure, and it was determined that the product was the target product [Dy 4 (C 15 h 15 N 4 O) 4 (μ 2 -OH) 4 ]·4ClO 4 -. Characterization of the magnetic properties of the obtained product shows that the obtained product has a single-molecule magnet behavior.

Embodiment 3

[0068] Repeat Example 1, the difference is:

[0069] 1) After adding 1mL of aldehyde-amine mixture to the glass bottle, add 2mL of acetonitrile to it, so that the volume ratio of ethanol and acetonitrile in the mixed solvent is 1:5;

[0070] 2) adjust the pH of the system to 8.3 with triethylamine;

[0071] 3) The reaction is carried out at 30° C., and the reaction time is 20 h.

[0072] Colorless crystals with long strips and missing corners were obtained with a yield of 27.1%. The resulting product was characterized for its structure, and it was determined that the product was the target product [Dy 4 (C 15 h 15 N 4 O) 4 (μ 2 -OH) 4 ]·4ClO 4 - . Characterization of the magnetic properties of the obtained product shows that the obtained product has a single-molecule magnet behavior.

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Abstract

The invention discloses a 2-pyridinecarboxaldehyde-1,3-diamino-2-propanol Schiff base tetranuclear dysprosium cluster compound and a synthesis method and application thereof. The cluster compound belongs to a tetragonal system and an I-4 space group, and the chemical formula is [Dy4(C15H15N4O)4(mu2-OH)4] 4ClO4-. The synthesis method for the cluster compound includes the steps of dissolving pyridine-2-carboxaldehyde, 1,3-diamino-2-propanol and Dy(ClO4)3 6H2O in a mixed solvent, adjusting the pH of the obtained solution to 7.8-8.5, and reacting the obtained mixed solution without heating to precipitate out crystals, wherein the mixed solvent is a combination of ethanol and acetonitrile. The cluster compound has field-induced single-molecule magnet behaviors and can be used for preparing magnetic materials; the whole reaction is carried out without heating, conditions are controllable, the synthesis method is simple and easy to operate, the yield is high, and the reproducibility is good.

Description

technical field [0001] The invention relates to a 2-pyridine formaldehyde acetal 1,3 diamino-2-propanol Schiff base tetranuclear dysprosium cluster compound and a synthesis method and application thereof, belonging to the technical field of magnetic materials. Background technique [0002] Due to their structure and the unique properties of rare earth ions, rare earth complexes have excellent optical, electrical, and magnetic properties, and have broad application prospects in the fields of magnetic materials, optical sensors, and molecular recognition. Compared with transition metals, rare earth ions are often used to construct single-molecule magnets due to their large anisotropy, and their complexes often have excellent magnetic properties. In view of the excellent magnetic properties of their complexes, researchers are currently Many rare earth complexes with single-molecule magnet behavior have been reported, ranging from mononuclear to hypernuclear. High-nuclear compl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/00H01F1/42
CPCC07F5/003H01F1/42
Inventor 邹华红付小小梁福沛
Owner GUANGXI NORMAL UNIV
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