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2-aldehyde-8-hydroxyquinoline-1,3-diamino-2-propyl alcohol Schiff base four-core dysprosium cluster compound and synthesis method thereof

A technology of hydroxyquinoline and synthesis method, which is applied in the direction of 3/13 group organic compounds without C-metal bond, compounds containing periodic table group 3/13 elements, chemical instruments and methods, etc., can solve the inconvenient modeling Calculation and other problems, to achieve the effect of simple and easy operation of the synthesis method

Active Publication Date: 2018-11-20
山东顺创新材料科技有限公司
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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, it has not been seen that 2-formyl-8-hydroxyquinoline and 1,3-diamino-2-propanol are spontaneously assembled to form ligands in situ and then combined with Dy(NO 3 ) 3 ·6H 2 A related report of 2-formyl-8-hydroxyquinoline-1,3-diamino-2-propanol Schiff base tetranuclear dysprosium cluster obtained by O reaction

Method used

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  • 2-aldehyde-8-hydroxyquinoline-1,3-diamino-2-propyl alcohol Schiff base four-core dysprosium cluster compound and synthesis method thereof
  • 2-aldehyde-8-hydroxyquinoline-1,3-diamino-2-propyl alcohol Schiff base four-core dysprosium cluster compound and synthesis method thereof
  • 2-aldehyde-8-hydroxyquinoline-1,3-diamino-2-propyl alcohol Schiff base four-core dysprosium cluster compound and synthesis method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1) Weigh 0.173g (1mmol) of 2-formyl-8-hydroxyquinoline and dissolve it in 5mL of anhydrous acetonitrile, and dissolve 0.0456g (0.05mmol) of 1,3-diamino-2-propanol in 5mL of ethanol, After completely dissolving, slowly add the acetonitrile solution of 2-formyl-8-hydroxyquinoline into the ethanol solution of 1,3-diamino-2-propanol, mix well to obtain a mixed solution, and set aside;

[0026] 2) Weigh the metal salt Dy(NO 3 ) 3 ·6H 2 O (0.1mmol, 45.6mg) was added to a glass bottle with a volume of about 20mL, and 1mL of the above-mentioned aldehyde-amine mixture was drawn into the glass bottle with a pipette gun, and then 0.5mL of ethanol and 2.5mL of acetonitrile were added to it, so that The volume ratio of ethanol and acetonitrile in the glass bottle is 1:3 (1mL and 3mL respectively), then add 15μL triethylamine to it, shake well (the pH of the solution at this time=9.6); then seal the glass with aluminum foil Bottle mouth, cover the bottle cap, place the glass bottl...

Embodiment 2

[0062] Repeat Example 1, the difference is:

[0063] 1) After adding 1mL of aldehyde-amine mixture into the glass bottle, add 0.5mL of ethanol and 3.5mL of acetonitrile to it, so that the volume ratio of ethanol and acetonitrile in the mixed solvent is 1:4;

[0064] 2) adjust the pH of the system to 9.8 with triethylamine;

[0065] 3) The reaction is carried out at 50° C., and the reaction time is 48 hours.

[0066] Red long strip crystals were obtained with a yield of 21.7%. The resulting product was characterized for its structure, and it was determined that the product was the target product [Dy 4 (C 23 h 17 N 4 o 3 ) 2 (μ 3 -OH) 2 (NO 3 ) 4 (H 2 O) 2 ]. 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 into the glass bottle, add 0.5mL of ethanol and 4.5mL 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 9.5 with triethylamine;

[0071] 3) The reaction is carried out at 80° C., and the reaction time is 30 h.

[0072] Red long strip crystals were obtained with a yield of 23.9%. The resulting product was characterized for its structure, and it was determined that the product was the target product [Dy 4 (C 23 h 17 N 4 o 3 ) 2 (μ 3 -OH) 2 (NO 3 ) 4 (H 2 O) 2 ]. 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-aldehyde-8-hydroxyquinoline-1,3-diamino-2-propyl alcohol Schiff base four-core dysprosium cluster compound and a synthesis method thereof. The cluster compound belongs to amonoclinic system, a P21 / n space group, and the chemical formula is [Dy4(C23H17N4O3)2(mu3-OH)2(NO3)4(H2O)2]. The synthesis method of the cluster compound comprises the following steps: dissolving 2-aldehyde-8-hydroxyquinoline, 1,3-diamino-2-propyl alcohol and Dy(NO3)3*6H2O into a mixed solvent, adjusting the pH of the obtained solution to be 9.4 to 10.0, performing reaction on the obtained mixedliquid under the heating condition, cooling a reactant and separating out crystals to obtain the cluster compound, wherein the mixed solvent is a composition of ethanol and acetonitrile. The cluster compound has field induced single-molecular magnet behavior and can be used for preparing a magnetic material; furthermore, the synthesis method is simple and easy to operate.

Description

technical field [0001] The invention relates to a 2-formyl-8-hydroxyquinoline-1,3-diamino-2-propanol Schiff base tetranuclear dysprosium cluster compound and a synthesis method 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 complexes often have com...

Claims

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Application Information

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IPC IPC(8): C07F5/00H01F1/42
CPCC07F5/003H01F1/42
Inventor 邹华红付小小梁福沛
Owner 山东顺创新材料科技有限公司
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