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. problems such as the loss of sexual catalysts

Active Publication Date: 2020-02-04
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, at room temperature, disperse montmorillonite in water with 5 times the mass, stir evenly, add sodium hydroxide with 5% mass of montmorillonite, and stir for 2 hours. The bentonite is a chemically pure product, and the water is Deionized water with a conductivity equal to 8 μS / cm;

[0022] In the second step, filter the above-mentioned montmorillonite, wash with the water used in the first step until neutral, dry at 70°C, and set aside;

[0023] The 3rd step, under room temperature, take transition metal salt and dissolve in the water of its 3 times of mass, described transition metal salt is chemical pure reagent, and its cation is iron ion (III), and its anion is chloride ion, and the first solvent is chemical pure water;

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

[0025] In the fifth st...

Embodiment 2

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

[0031] In the second step, filter the above-mentioned montmorillonite, wash with the water used in the first step until neutral, dry at 70°C, and set aside;

[0032] The 3rd step, under room temperature, get transition metal salt and dissolve in the water of its 5 times of mass, described transition metal salt is analytical pure reagent, and its cation is manganese ion (II), and its anion is bromide ion, and the first solvent is analytical reagent. pure water;

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

Embodiment 3

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

[0040] In the second step, filter the above-mentioned montmorillonite, wash with the water used in the first step until neutral, dry at 80°C, and set aside;

[0041] In the third step, at room temperature, a transition metal salt is dissolved 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 a sulfate radical. The first solvent is analytically pure water;

[0042] In the fourth step, another chiral compound is dissolved in the second solvent with 5 times its mass, and the chiral compound is analytically pure 3-(S)-(1-formamido-1,1-diphenylmethyl ) pyrrolidine, the second...

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Abstract

The invention relates to a montmorillonite immobilized chiral compound and a preparation method thereof. The preparation method comprises: dispersing montmorillonite in water, adding sodium hydroxide,stirring, filtering, washing to be neutral, and drying; taking a transition metal salt, dissolving in water, taking a chiral compound, and dissolving in a second solvent; adding the prepared chiral compound solution into the transition metal salt solution; adding water into the prepared montmorillonite, uniformly stirring, and adding the metal cooperation compound into the montmorillonite suspension in a dropwise manner; filtering, and cooling to obtain the product. According to the invention, the product is stable in immobilization, and the immobilized chiral compound cannot be detected in asolution after being washed more than 100 times with a liquid chromatographically pure solvent.

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 closely related to life. In recent years, people's demand for single-chiral compounds (such as chiral medicines and pesticides, etc.) 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-catalyzed synthesis are three methods for obtaining chiral substances, among which chiral catalysis is the most effective method because it can achieve chiral proliferation. An efficient chiral catalyst molecule can induce tens of thousands or even millions of chiral product molecules, reaching or even exceeding the level of enzyme ...

Claims

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Application Information

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Patent Type & Authority Applications(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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