2-pyridinecarboxaldehyde-1,3-diamino-2-propanol Schiff base tetranuclear dysprosium cluster compound and synthesis method and application thereof
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., and can solve the inconvenient modeling calculation. and other problems, to achieve the effect of simple and easy operation of the synthesis method, controllable conditions and low production cost
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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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