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

Active Publication Date: 2022-03-08
LANZHOU UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It effectively solves the technical problems of long reaction time and high catalyst loading in the three-component aza-Darzens reaction of existing different complex catalysts

Method used

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Experimental program
Comparison scheme
Effect test

preparation example Construction

[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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Abstract

The invention belongs to the technical field of homogeneous catalysis, and discloses a preparation method of a 3d-4f bionic metal cage, which comprises the following steps: (1) mixing an H5L ligand, methanol and triethylamine, and reacting to obtain a suspension A; (2) adding ZnCl2 into the suspension A, mixing and reacting to obtain a suspension B; and (3) mixing rare earth nitrate, methanol and the suspension B, and reacting to obtain the 3d-4f bionic metal cage. The method is simple in step operation, industrial preparation can be realized, and the prepared 3d-4f bionic metal cage has very high catalytic activity in catalysis of a three-component aza-Darzens reaction.

Description

technical field [0001] The invention relates to the technical field of homogeneous catalysis, in particular to a 3d-4f bionic metal cage and its preparation method and application. Background technique [0002] As a kind of Darzens reaction, the aza-Darzens reaction is widely used in the synthesis of various minimal saturated nitrogen heterocyclic compounds with biological activity, and it is also a useful precursor of other nitrogen-containing compounds, which can be realized by nucleophilic ring-opening reaction or other reactions transform. Although a variety of synthetic strategies can effectively prepare aziridine derivatives, most of the methods usually have the problem of expensive starting materials or cumbersome synthetic steps. At present, there are few studies on the three-component aza-Darzens reaction. The application of tetrahedral Ga(III) as a nanoreactor and Zr-MOF as a heterogeneous catalyst in this type of reaction confirms that it is an effective method f...

Claims

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Application Information

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IPC IPC(8): C07F3/06B01J31/22C07D203/02C07D203/08
CPCC07F3/06C07F3/003B01J31/2217C07D203/02C07D203/08B01J2531/26B01J2531/38Y02E60/36
Inventor 唐晓亮周生斌窦伟刘伟生
Owner LANZHOU UNIVERSITY
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