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Preparation method of new material for separating and purifying chiral tetramisole (TM)

A technology of tetramisole and new materials, which is applied in the field of preparation of new materials for the separation and purification of chiral tetramisole, can solve the problems of low efficiency of surface imprinted materials, and achieve good selectivity, recognition and binding, and material utilization High, the effect of improving mechanical strength

Inactive Publication Date: 2011-09-14
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to solve the problem of low efficiency of the surface imprinted material for separating L-TM, the present invention provides a preparation method for a new material used for the separation and purification of chiral tetramisole

Method used

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  • Preparation method of new material for separating and purifying chiral tetramisole (TM)
  • Preparation method of new material for separating and purifying chiral tetramisole (TM)
  • Preparation method of new material for separating and purifying chiral tetramisole (TM)

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Effect test

Embodiment 1

[0034] The preparation method of the new material used for separation and purification of chiral tetramisole comprises the following steps:

[0035] 1. Chemical surface modification of silica gel: Add 10g of activated silica gel to 120ml of water, and add 15ml of aminosilane coupling agent γ-aminopropyltrimethoxysilane (also can be γ-aminopropyltriethoxysilane) , reacted at 50 ° C for 20 h, and the product after suction filtration was washed repeatedly with ethanol and dried in vacuum to obtain surface-modified silica gel particles AMPS-SiO 2 ;

[0036] 2. Chemical grafting of polymethacrylic acid on the surface of silica gel particles: add 1 g of modified silica gel particles AMPS-SiO to a four-necked flask 2 , then add 80mL of water and 5mL of monomeric methacrylic acid, pass nitrogen for 30min to remove the air in the system, then raise the temperature of the system to 40°C, add 1.1% initiator ammonium persulfate whose mass is the mass of the monomer, and Carry out graft ...

Embodiment 2

[0039] The preparation method of the new material used for separation and purification of chiral tetramisole comprises the following steps:

[0040] 1. Chemical surface modification of silica gel: Add 15g of activated silica gel to 100ml of water, and add 10ml of aminosilane coupling agent N-β(aminoethyl)-γ-aminopropyltrimethoxysilane (also can be N- β(aminoethyl)-γ-aminopropylmethyldimethoxysilane, N-β(aminoethyl)-γ-aminopropyltriethoxysilane, or N-β(aminoethyl)- γ-aminopropylmethyldiethoxysilane), reacted at 50°C for 22h, the product after suction filtration was repeatedly washed with ethanol, and dried in vacuum to obtain surface-modified silica gel particles AMPS-SiO 2 ;

[0041] 2. Chemical grafting of polymethacrylic acid on the surface of silica gel particles: add 1.5g of modified silica gel particles AMPS-SiO to a four-necked flask 2 , then add 90mL of water and 4.5mL of monomer methacrylic acid, pass nitrogen gas for 30min to remove the air in the system, then raise...

Embodiment 3

[0044] The preparation method of the new material used for separation and purification of chiral tetramisole comprises the following steps:

[0045] 1. Chemical surface modification of silica gel: add 13g of activated silica gel to 150ml of water, and add 13ml of aminosilane coupling agent anilinomethyltrimethoxysilane (also can be anilinomethyltriethoxysilane, or ammonia Ethylaminopropyltrimethoxysilane), reacted at 50°C for 24h, the product after suction filtration was repeatedly washed with ethanol, and dried in vacuum to obtain surface-modified silica gel particles AMPS-SiO 2 ;

[0046] 2. Chemical grafting of polymethacrylic acid on the surface of silica gel particles: add 1.2g of modified silica gel particles AMPS-SiO to a four-neck flask 2 , then add 100mL of water and 4mL of monomer methacrylic acid, pass nitrogen gas for 30min to remove the air in the system, then raise the temperature of the system to 40°C, add 1.2% initiator ammonium persulfate whose mass is the mo...

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Abstract

The invention discloses a preparation method of a new material for separating and purifying chiral tetramisole (TM), which is used for solving the problem of low efficiency of the existing surface imprinted material for separating L-TM. The preparation method comprises the following steps: activating silica gel particles, and connecting the surfaces of the silica gel particles with an amino-containing silane coupling agent through chemical bonds; chemically grafting the surfaces of the silica gel particles with polymethylacrylic acid; and preparing a silica gel particle surface molecular imprinted polymer (SMIP). In the method, the silica gel particles are taken as a carrier, methacrylic acid is taken as a functional macromolecular material grafted with the surfaces of the particles or microspheres, and the amino-containing silane coupling agent is taken as a cross-linking agent to obtain the surface imprinted material which has the advantages of fast binding speed, strong recognitionand selectivity and high binding capacity on L-TM molecules. The surface imprinted material prepared by the method has the advantages of high material utilization ratio, low cost, and good selectivity and recognition and associativity on the L-TM molecules, thus meeting the requirements for industrial production.

Description

technical field [0001] The invention relates to a preparation method of a new material used for separation and purification of chiral tetramisole. Background technique [0002] Modern pharmacology has proved that the chirality of a drug is closely related to its efficacy. After different optical isomers of the same drug enter the living body, there are often significant differences in their biological activity, metabolism, efficacy and side effects. Therefore, trying to obtain optically pure chiral drugs to obtain new drugs with high efficacy has become an important development goal of medical science. Optically pure chiral drugs can be prepared by chiral source synthesis and asymmetric synthesis, but due to the limited types of natural chiral substances and the technical difficulties of asymmetric synthesis, the resolution of racemates becomes an important task to obtain optically pure chiral drugs. The most important route for homochiral compounds. Among the drugs curren...

Claims

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Application Information

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IPC IPC(8): C08F292/00C08J9/26C08J3/24B01J20/26B01J20/28B01J20/30
Inventor 高保娇安富强杜瑞奎王蕊欣
Owner ZHONGBEI UNIV
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