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A kind of spiral polymer functionalized silica microsphere chiral stationary phase and its preparation and application

A technology of chiral stationary phase and silica gel microspheres, which is applied in the direction of alkali metal compounds, chemical instruments and methods, alkali metal oxides/hydroxides, etc., and can solve the problems of inability to separate and identify chiral compounds, backwardness, and differences in distribution and metabolism And other issues

Active Publication Date: 2022-08-09
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although chiral isomers have similar physical and chemical properties, they show great differences in distribution, metabolism, etc. in organisms
For example, in the famous "thalidomide (thalidomide)" incident, due to the backwardness of science and technology at that time, people did not fully understand the differences between chiral enantiomers, and could not separate and identify chiral compounds, which led to this huge tragedy.

Method used

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  • A kind of spiral polymer functionalized silica microsphere chiral stationary phase and its preparation and application
  • A kind of spiral polymer functionalized silica microsphere chiral stationary phase and its preparation and application
  • A kind of spiral polymer functionalized silica microsphere chiral stationary phase and its preparation and application

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Embodiment

[0026] Preparation of hand -fixed phase:

[0027] 1) Activation of silicon microspheres: Take 1.0G silicon microspheres (2.9-3.2 μm) scattered in 30 mL hydrochloric acid solution (3mol L (3mol L) under the action of ultrasound. -1 ) In the middle of 110 ° C, the reflux reaction was 12h. Use the sand core funnel to filter the silicon pipe, and use ultra -pure water and methanol to wash silicon balls in turn, and then dry it in a vacuum drying box of 80 ° C for 24h;

[0028] 2) Silicon microsphere surface connection: Take step 1) 1.0g in the 1.0G has been activated to the 30ml dry toluene under ultrasound, add 0.6g of Silicidine O- The base) -N- (triangular oxyxyxanel propylene) amino methyl acid ester, 100 μL water-free triamine, and reaches the reaction of 24h at 120 ° C through nitrogen protection. After the reaction is over, stir and cool to room temperature, and then use toluene and methanol to wash the silicon balls in turn, and dry it in a vacuum drying box at 100 ° C for 24h...

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Abstract

The invention relates to the preparation of a helical polymer-functionalized silica gel microsphere chiral stationary phase (Chiral Separation Phase, CSP) and its application in chiral separation. Specifically, an alkynyl group is first introduced on the surface of the silica gel microspheres, and then a functional monomer (Fmoc-L-phenylalanine derivative) and a catalyst are added, and the monomer can undergo "alkynyl-alkynyl" addition under the action of the catalyst. A helical structure is formed through a polymerization reaction, thereby preparing a surface-modified helical polymer silica microsphere material. Since the functional monomer, Fmoc‑L‑phenylalanine derivative, itself has a chiral structure, the material can be used as a chiral Stationary phases are used for the separation of chiral compounds. The preparation process of the chiral stationary phase is simple, the reaction conditions are mild, and it can be used for large-scale preparation.

Description

Technical field [0001] The present invention involves the separation of the refinery. After modifying the surface of the silicon dioxide microspheres 3-巯 巯 炔 炔, add the function of the chemical reactive function and the catalyst. The polymer function of the polymer function of the spiral structure to the surface of the silicon ball to form a silicon -sophilic silicon microsphere of a single molecule function of the single molecular function of the single molecular function. Disassembling to refine. Background technique [0002] Hand nature is considered to be one of the key structural factors that perform a series of complex functions in nature, and exist in the biological process. Among them, spirals are one of its simplest and most important states. For example, the polypeptide chain that compose a protein and the deoxyucleotide that constitutes the DNA chain has a spiral structure. The discovery of the spiral structure has aroused the attention of scientists to synthesize the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/29B01J20/285B01J20/28B01D15/38
CPCB01J20/29B01J20/285B01J20/28021B01D15/3833Y02P20/55
Inventor 马淑娟王妍欧俊杰叶明亮
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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