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Chiral oxidation catalyst and preparation method thereof

An oxidation catalyst, chiral technology, applied in physical/chemical process catalysts, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., can solve problems such as enantiomeric drug pollution

Inactive Publication Date: 2012-05-09
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Many opportunities and challenges in this field come from drug research, and now people are more and more aware of the importance of single enantiomers, the wrong use of enantiomers in racemic drugs is a serious drug contamination, which may cause Unpredictable toxic side effects such as reaction stop has two configurations of R and S, in which the R-isomer is an effective sedative, but the S-configuration is a strong teratogenic agent

Method used

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  • Chiral oxidation catalyst and preparation method thereof
  • Chiral oxidation catalyst and preparation method thereof
  • Chiral oxidation catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A. Add 0.01mol zinc nitrate hexahydrate, 0.005mol aluminum nitrate nonahydrate and 0.035mol urea into 320ml deionized water, dissolve and transfer to a 500ml three-necked flask, stir and heat to reflux for 24 hours. After the reaction, the product was suction filtered, washed with deionized water until the pH was 7, then washed once with ethanol to disperse the product evenly, and the filter cake was dried in an oven at 60°C to obtain a solid powder, which was Zn-Al-CO 3 -LDHs

[0022] B. Will get Zn-Al-CO 3 0.4g of LDHs was added to NaNO dissolved in 1.5mol / L 3 solution, add 0.002mol concentrated HNO 3 , N 2 protection, stirred and crystallized at room temperature for 24 hours, after the reaction, the product was suction filtered, washed with deionized water until the pH was 7, then washed once with ethanol to make the product evenly dispersed, and the filter cake was dried in an oven at 25°C to obtain a solid powder, namely Zn-Al-NO 3 - LDHs precursors.

[0023]...

Embodiment 2

[0027] A. take step A method in the similar embodiment 1 to obtain Zn-Al-CO 3 -LDHs.

[0028] B. Obtain Zn-Al-NO by the method of step B among the similar embodiment 1 3 -LDHs precursor

[0029] C. the pH value of L-glutamic acid is adjusted to 12 with the NaOH solution of 2mol / l, and preparation concentration is the negatively charged L-glutamic acid anion solution of 0.086mol / l, adds hydrotalcite precursor 0.15g, in 60℃ in N 2 The reaction was carried out for 12h under protection and stirring, and the product was used to remove CO 2 Washing with water, fully washing with absolute ethanol water, centrifuging, and vacuum drying at 25°C to obtain intercalated L-glutamic acid intercalated hydrotalcite, and then stored under dry conditions.

[0030] D. Add 50μl VO(O-i-Pr) 3 Add 1ml of dichloromethane to obtain a solution with a concentration of 0.5mol / L, then add the L-glutamic acid intercalation hydrotalcite prepared by C to the above solution, stir at 40°C for 1 hour, and ...

Embodiment 3

[0033] A. take step A method in the similar embodiment 1 to obtain Zn-Al-CO 3 -LDHs.

[0034] B. Obtain Zn-Al-NO by the method of step B among the similar embodiment 1 3 -LDHs precursor

[0035] C. Adjust the pH value of L-glutamic acid to 10 with concentrated ammonia water, and prepare a negatively charged L-glutamic acid anion solution with a concentration of 0.3mol / l, add 0.15g of hydrotalcite precursor, and put it under N at 20°C 2 The reaction was carried out for 48h under protection and stirring, and the product was used to remove CO 2 Washing with water, fully washing with absolute ethanol water, centrifuging, and vacuum drying at 25°C to obtain intercalated L-glutamic acid intercalated hydrotalcite, and then stored under dry conditions.

[0036] D. Add 25μl VO(O-i-Pr) 3 Add 1ml of dichloromethane to obtain a solution with a concentration of 0.1mol / L, then add the L-glutamic acid intercalation hydrotalcite prepared by C to the above solution, and stir at 10°C for 5h...

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Abstract

The invention relates to a chiral oxidation catalyst and a preparation method thereof, belonging to the technical field of catalyst synthesis. The chiral oxidation catalyst has a chemical composition general formula of [M<2+>1-xM<3+>x(OH)2]x+[(Glua-)b(CO3<2->)c]*mH2O. The preparation method comprises the following steps of: preparing a hydrotalcite precursor with interlayer anions of NO<3-> and the mol ratio of divalent and trivalent cations of a laminated plate: M<2+> / M<3+>=2 to 4; adjusting a pH value of alkali liquor to be 8-12, preparing to obtain a negatively charged amino acid anion solution with the concentration of 0.005-0.30 mol / L, adding to the hydrotalcite precursor with the interlayer anions of NO<3->, reacting while stirring at 20-60 DEG C for 12-48 h under the protection of N2, washing the product with CO2 water, fully washing with absolute ethyl alcohol water, centrifuging, recovering the solid product, drying at 30-50 DEG C in vacuum and adding the prepared intercalation amino acid hydrotalcite to 1-4 ml of dichloromethane solution; and then, adding a vanadium compound and stirring at 10-40 DEG C for 1-5 h to obtain a chiral oxidation catalyst. The invention has the advantages that the selectivity of reaction products is improved while a relatively high yield is kept.

Description

technical field [0001] The invention belongs to the technical field of catalyst synthesis, and in particular provides a chiral oxidation catalyst and a preparation method thereof. Background technique [0002] Asymmetric catalysis has made remarkable achievements in the past few decades, so the 2001 Nobel Prize in Chemistry was awarded to Knowles, Noyori and Sharpless, who were engaged in the synthesis of asymmetric catalysis, in recognition of their outstanding achievements in this field contribute. Many opportunities and challenges in this field come from the research of drugs, and now people are more and more aware of the importance of single enantiomers, the wrong use of enantiomers in racemic drugs is a serious drug contamination, which may cause Unpredictable toxic side effects such as reaction stop has R, S two configurations, wherein the R-isomer is an effective sedative, but the S-configuration is a strong teratogenic agent. Single enantiomeric chiral compounds ca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/26C07D301/19C07D303/14
Inventor 何静王玖钊
Owner BEIJING UNIV OF CHEM TECH
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