3d-4f bionic metal cage and preparation method and application thereof
A 3d-4f, metal cage technology, applied in the direction of 2/12 organic compounds without C-metal bonds, chemical instruments and methods, organic compound/hydride/coordination complex catalysts, etc., can solve the problem of catalyst loading High, long reaction time and other problems, to achieve the effect of high catalytic activity, simple preparation method, high yield
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[0024] The invention provides a kind of preparation method of 3d-4f bionic metal cage, comprises the following steps:
[0025] (1) H 5 L ligand, methanol and triethylamine are mixed and reacted to obtain suspension A;
[0026] (2) ZnCl 2 Add to Suspension A, mix and react to obtain Suspension B;
[0027] (3) react after mixing rare earth nitrate, methanol and suspension B to obtain 3d-4f biomimetic metal cage;
[0028] Among them, H 5 The structural formula of the L ligand is as follows:
[0029] .
[0030] As a preference, the H 5 The preparation method of L ligand is as follows:
[0031] S1. Under protective gas, react after mixing ethyl glycine hydrochloride, triethylamine, anhydrous dichloromethane and monoethyl oxalyl chloride solution to obtain 3-((2-ethoxyl-2-oxo Ethyl)amino)-3-oxopropionic acid ethyl ester;
[0032] S2, react after mixing 3-((2-ethoxy-2-oxyethyl)amino)-3-oxopropionic acid ethyl ester, hydrazine hydrate and ethanol to obtain 2-hydrazino-N-(2 ...
Embodiment 1
[0059] 23.6mg H 5 L ligand, 4mL methanol and 16μL triethylamine were placed in a 25mL round bottom flask, stirred at room temperature for 10 minutes to obtain a light yellow suspension A; then 6.8mg ZnCl 2 Add to suspension A, stir at room temperature for 10 minutes to obtain yellow suspension B; then add 22.2 mg of lanthanum nitrate to suspension B, stir at room temperature for 5 minutes, add 3 mL of methanol, continue stirring for 30 minutes and filter , and evaporate at room temperature. Two weeks later, light yellow blocky crystals suitable for crystal analysis were obtained, washed three times with cold methanol, and dried in air to obtain 3d-4f biomimetic metal cages. The calculated yield of the 3d-4f biomimetic metal cage of this embodiment is 56.8%.
Embodiment 2
[0061] 21.8mg H 5 L ligand, 4mL methanol and 17μL triethylamine were placed in a 25mL round bottom flask, stirred at room temperature for 8 minutes to obtain a light yellow suspension A; then 7.3mg ZnCl 2 Add to suspension A, stir at room temperature for 8 minutes to obtain yellow suspension B; then add 20.9 mg of samarium nitrate to suspension B, stir at room temperature for 5 minutes, add 4 mL of methanol, continue stirring for 35 minutes and filter , and evaporate at room temperature. Two weeks later, light yellow blocky crystals suitable for crystal analysis were obtained, washed three times with cold methanol, and dried in air to obtain 3d-4f biomimetic metal cages. The calculated yield of the 3d-4f biomimetic metal cage of this embodiment is 54.6%.
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