A kind of montmorillonite immobilized chiral compound and preparation method thereof

A chiral compound, montmorillonite technology, applied in chemical instruments and methods, catalyst activation/preparation, organic compound/hydride/coordination complex catalysts, etc., can solve chiral center racemization, small loading force , easy desorption and other problems

Active Publication Date: 2022-07-12
XI'AN PETROLEUM UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above-mentioned loading technology, the force of loading by means of physical adsorption is small, and it is easy to desorb, resulting in the loss of the chiral catalyst; the reaction by establishing a new C-C bond is complicated, and there are problems such as racemization of the chiral center during the reaction process.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The first step is to disperse the montmorillonite in 5 times the mass of water at room temperature, stir evenly, add 5% sodium hydroxide by mass of the montmorillonite, and stir for 2 hours. The bentonite is a chemically pure product, and the water is Deionized water with conductivity equal to 8 μS / cm;

[0022] In the second step, the above-mentioned montmorillonite was filtered, washed with the water used in the first step until neutral, dried at 70°C, and used for later use;

[0023] In the third step, at room temperature, dissolve a transition metal salt in water of 3 times its mass, the transition metal salt is a chemically pure reagent, its cation is iron ion (III), its anion is chloride ion, and the first solvent is chemical pure water;

[0024] In the fourth step, another chiral compound is taken and dissolved in the second solvent of 7 times of its mass, the chiral compound is chemically pure L-proline, and the second solvent is chemically pure water;

[0025]...

Embodiment 2

[0030] The first step is to disperse the montmorillonite in 6 times the mass of water at room temperature, stir evenly, add 8% sodium hydroxide by mass of the montmorillonite, and stir for 4 hours, the bentonite is an analytically pure product, and the water is the conductivity deionized water with a rate equal to 5 μS / cm;

[0031] In the second step, the above-mentioned montmorillonite was filtered, washed with the water used in the first step until neutral, dried at 70°C, and used for later use;

[0032] The third step, at room temperature, dissolve the transition metal salt in water of 5 times its mass, the transition metal salt is an analytical reagent, its cation is manganese ion (II), its anion is bromide ion, and the first solvent is analytical pure water;

[0033]In the fourth step, another chiral compound is taken and dissolved in a second solvent of 4 times its mass, the chiral compound is analytically pure (+)-L-tartrate dibenzylamide, and the second solvent is ana...

Embodiment 3

[0039] The first step, at room temperature, disperse the montmorillonite in 8 times the mass of water, stir evenly, add 10% sodium hydroxide by mass of the montmorillonite, and stir for 5 hours, the bentonite is a chemically pure product, and the water is an electrical conductivity deionized water with a rate equal to 5 μS / cm;

[0040] In the second step, the above-mentioned montmorillonite was filtered, washed with the water used in the first step until neutral, dried at 80°C, and used for later use;

[0041] The third step, at room temperature, take the transition metal salt and dissolve it in water of 6 times its mass, the transition metal salt is a reagent of chemical purity and above purity, its cation is iron ion (II), and its anion is sulfate radical, The first solvent is analytically pure water;

[0042] In the fourth step, take another chiral compound and dissolve it in the second solvent of 5 times its mass, the chiral compound is analytically pure 3-(S)-(1-carboxam...

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Abstract

The invention relates to a montmorillonite-immobilized chiral compound and a preparation method thereof. The montmorillonite-supported chiral compound is prepared by the following method: dispersing the montmorillonite in water, adding sodium hydroxide, stirring, filtering, washing to neutrality, and drying; dissolving the transition metal salt in water, and adding another Dissolving or dispersing the chiral compound in the second solvent; adding the prepared chiral compound solution to the transition metal salt solution; taking the prepared montmorillonite, adding water, stirring evenly, and adding the metal complex dropwise to the above montmorillonite Suspension; filter and cool. The product of the invention is stable in immobilization, and the immobilized chiral compound cannot be detected in the solution after washing with liquid chromatography pure solvent for more than 100 times.

Description

technical field [0001] The invention relates to the technical field of solid catalyst preparation, in particular to a method for immobilizing chiral compounds on montmorillonite. Background technique [0002] Chirality is one of the basic properties of nature and is closely related to life. In recent years, the demand for single chiral compounds (such as chiral medicines and pesticides) and chiral functional materials has promoted the vigorous development of chiral science. In addition to natural sources, artificial synthesis is the main way to obtain chiral substances. Racemate resolution, substrate-induced chiral synthesis and chiral catalytic synthesis are three methods to obtain chiral substances, among which, chiral catalysis is the most effective method because it can achieve chiral proliferation. An efficient chiral catalyst molecule can induce thousands or even millions of chiral product molecules, reaching or even exceeding the level of enzyme catalysis. So far, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22B01J31/24B01J37/30
CPCB01J31/1616B01J31/182B01J31/1805B01J31/2404B01J31/2217B01J31/2213B01J37/30B01J2531/0275B01J2531/0272B01J2531/0269B01J2531/842B01J2531/72B01J2531/845B01J2531/847B01J2531/16Y02P20/584
Inventor 汤颖徐中英周瑞李红吴亚
Owner XI'AN PETROLEUM UNIVERSITY
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