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2-pyridine-carboxaldehyde condensation 1,3-diamino-2-propanol Schiff base double-core dysprosium cluster compound, synthetic method and application thereof

A technology of pyridine formaldehyde and synthesis method, which is applied to the 3/13 group organic compounds without C-metal bonds, compounds containing group 3/13 elements of the periodic table, organic chemical methods, etc., which can solve the inconvenience of modeling calculations, etc. problem, to achieve the effect that the synthesis method is simple and easy to operate

Active Publication Date: 2018-11-02
GUANGXI NORMAL UNIV
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  • Summary
  • 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, it has not been seen that 2-pyridinecarbaldehyde and 1,3-diamino-2-propanol are spontaneously assembled by in situ reaction to form a C-N-C-C-C-N six-membered ring and then combined with Dy(NO 3 ) 3 ·6H 2 Reaction of O to get 1,3 diamino-2-propanol Schiff base dinuclear dysprosium clusters from 2-pyridine formaldehyde

Method used

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  • 2-pyridine-carboxaldehyde condensation 1,3-diamino-2-propanol Schiff base double-core dysprosium cluster compound, synthetic method and application thereof
  • 2-pyridine-carboxaldehyde condensation 1,3-diamino-2-propanol Schiff base double-core dysprosium cluster compound, synthetic method and application thereof
  • 2-pyridine-carboxaldehyde condensation 1,3-diamino-2-propanol Schiff base double-core dysprosium cluster compound, synthetic method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1) Weigh 0.1071g (1mmol) of 2-pyridinecarbaldehyde and dissolve it in 5mL of acetonitrile, and dissolve 0.0451g (0.5mmol) of 1,3-diamino-2-propanol in 5mL of ethanol. The acetonitrile solution of pyridine 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;

[0028] 2) Weigh the metal salt Dy(NO 3 ) 3 ·6H 2 Add O (0.1mmol, 45.6mg) 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 6 μL triethylamine to it, shake well (the pH of the solution at this time=7.5); then seal the glass bottle mouth with aluminum foil, Cover the bottle cap, place the glass bottle in an oven at 60°C for 24 hours, take it out, wrap it...

Embodiment 2

[0065] Repeat Example 1, the difference is:

[0066] 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;

[0067] 2) adjust the pH of the system to 7.2 with triethylamine;

[0068] 3) The reaction is carried out at 50° C., and the reaction time is 48 hours.

[0069] Colorless long strip crystals were obtained with a yield of 22.1%. The resulting product was characterized for its structure, and it was determined that the product was the target product [Dy2 (C 9 h 11 N 3 O) 2 (NO 3 ) 4 ]. Characterization of the magnetic properties of the obtained product shows that the obtained product has a single-molecule magnet behavior.

Embodiment 3

[0071] Repeat Example 1, the difference is:

[0072] 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;

[0073] 2) adjust the pH of the system to 7.6 with triethylamine;

[0074] 3) The reaction is carried out at 80° C., and the reaction time is 30 h.

[0075] Colorless long crystals were obtained with a yield of 21.5%. The resulting product was characterized for its structure, and it was determined that the product was the target product [Dy 2 (C 9 h 11 N 3 O) 2 (NO 3 ) 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-pyridine-carboxaldehyde condensation 1,3-diamino-2-propanol Schiff base double-core dysprosium cluster compound, a synthetic method and application thereof. The cluster compound belongs to a P21 / n space group of a monoclinic crystal system, and the chemical formula is [Dy2(C9H11N3O)2(NO3)4]. The synthetic method of the cluster compound comprises the following steps of:taking 2-pyridine-carboxaldehyde, 1,3-diamino-2-propanol and Dy(NO3)3.6H2O in a mixed solvent, regulating pH of the obtained solution to 7.2-7.8, reacting the mixed solution under a heating condition,cooling reactants to precipitate crystal and obtaining the cluster compound, wherein the mixed solvent is a composition of ethyl alcohol and acetonitrile. The cluster compound disclosed by the invention has a field-induced unimolecular magnet behavior, and can be used for preparing magnetic materials; the synthetic method is simple and easy in operation.

Description

technical field [0001] The invention relates to a 2-pyridine formaldehyde acetal 1,3 diamino-2-propanol Schiff base dinuclear dysprosium cluster compound and a synthesis method and application thereof, which belong 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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IPC IPC(8): C07F5/00H01F1/42
CPCC07B2200/13C07F5/003H01F1/42
Inventor 邹华红付小小梁福沛
Owner GUANGXI NORMAL UNIV
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