Dysprosium complex constructed with 8-hydroxyquinoline acylhydrazone derivative as a ligand and its synthesis method and application
A technology of hydroxyquinoline acylhydrazone and a synthetic method, which is applied in the fields of organic chemistry, magnetism of organic materials/organic magnetic materials, organic chemistry, etc., can solve problems such as no unified explanation of the magnetic action mechanism of single-molecule magnets, and achieve synthesis Simple method, good repeatability and low cost
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Embodiment 1
[0034] Take the ligand 2-formyl-8-hydroxyquinoline-2-chloro-benzoylhydrazone (0.025mmol, 8.1mg) and Dy(NO 3 ) 3 ·6H 2O (0.025mmol, 11.4mg), was added to a Pyrex tube with a length of about 18cm that was closed at one end, and 0.9mL of CH 3 OH and 0.3mL H 2 O, add 1 drop of triethylamine dropwise, shake gently (the pH of the solution at this time = 8.1), seal the other end of the tube under vacuum conditions, and then keep it at 80°C for 72 hours, take it out, and use Cotton wool wrapped the Pyrex tube tightly and let it cool down to room temperature slowly, and dark red strip crystals were precipitated, with a yield of about 17% (calculated by Dy). Elemental analysis (%) (C 34 h 21 Cl 2 DyN 6 o 4 ), experimental value: C, 50.28, H, 2.74, N, 10.35; theoretical value: C, 50.35, H, 2.61, N, 10.36.
[0035] The product obtained in Example 1 is characterized:
[0036] 1) Infrared characterization:
[0037] Use American Nicolet 360 FT-IR type Fourier transform infrared sp...
Embodiment 2
[0057] Repeat Example 1, the difference is:
[0058] 1) The ratio of methanol and water in the mixed solvent is 2:1, and the total amount of the mixed solvent remains unchanged;
[0059] 3) Adjust the pH value of the solution to 8.2.
[0060] Take out the Pyrex tube, wrap the Pyrex tube tightly with cotton wool and let it cool down to room temperature slowly, deep red strip crystals are precipitated at the bottom of the Pyrex tube. Yield 22%.
[0061] The resulting product was characterized for its structure, and it was determined that the product was the target product [Dy(HL)(L)], wherein L was 2-formyl-8-hydroxyquinoline-2-chloro-benzoylhydrazone to remove the hydroxyl hydrogen atom and A hydrogen atom on the acylhydrazone nitrogen carries two units of negative charge; HL is 2-formyl-8-hydroxyquinoline-2-chloro-benzoylhydrazone, which removes the hydroxyl hydrogen atom and carries one unit of negative charge.
[0062] Characterization of the magnetic properties of the ob...
Embodiment 3
[0064] Repeat Example 1, the difference is:
[0065] 1) The ratio of methanol and water in the mixed solvent is 1:3, and the total amount of the mixed solvent remains unchanged;
[0066] 2) adjust the pH value of the solution to 8.3;
[0067] 3) Change the reaction temperature to 60°C and the reaction time to 80h.
[0068] Take out the Pyrex tube, wrap the Pyrex tube tightly with cotton wool and let it cool down to room temperature slowly, deep red strip crystals are precipitated at the bottom of the Pyrex tube. Yield 25%.
[0069] The resulting product was characterized for its structure, and it was determined that the product was the target product [Dy(HL)(L)], wherein L was 2-formyl-8-hydroxyquinoline-2-chloro-benzoylhydrazone to remove the hydroxyl hydrogen atom and A hydrogen atom on the acylhydrazone nitrogen carries two units of negative charge; HL is 2-formyl-8-hydroxyquinoline-2-chloro-benzoylhydrazone, which removes the hydroxyl hydrogen atom and carries one unit ...
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