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A chiral stationary phase bonded with amylose derivatives and its preparation method

A technology of chiral stationary phase and amylose, applied in chemical instruments and methods, and other chemical processes, can solve the problems of insufficient chiral selectivity and instability, and achieve good selectivity, stability, and excellent The effect of chiral selectivity

Active Publication Date: 2016-09-07
NANTONG HONGYU ANALYTICAL INSTR
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a chiral stationary phase bonded with amylose derivatives to solve the technical problems of polysaccharide chiral columns unstable under alkaline conditions and insufficient chiral selectivity in the prior art

Method used

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  • A chiral stationary phase bonded with amylose derivatives and its preparation method
  • A chiral stationary phase bonded with amylose derivatives and its preparation method
  • A chiral stationary phase bonded with amylose derivatives and its preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0034] The preparation of the chiral stationary phase bonded with amylose derivatives, the specific process is as follows:

[0035] Step 1: Take 10g of styrene-divinylbenzene polymer-coated silica gel and add 300mL of concentrated hydrochloric acid and water with a volume ratio of 1:1. Under electromagnetic stirring, heat and reflux in an oil bath at 90°C for 4h, cool, stand still, and pour out Acid solution, washed several times with water until it becomes neutral; after drying, add 70mL toluene and 1g aminopropyltriethoxysilane, react at 100°C for 24h, add 15mL trimethylchlorosilane for reaction, and use After washing and drying with toluene, diethyl ether and methanol, a styrene-divinylbenzene polymer-coated silica gel containing aminopropyl groups on the surface is prepared. The number of aminopropyl groups on the surface of styrene-divinylbenzene polymer coated silica gel is controlled by the amount of trimethylchlorosilane to 0.8 μmol / m 2 .

[0036] Step 2: Suspend 1g ...

Embodiment 2

[0045]The preparation of the chiral stationary phase bonded with amylose derivatives, the specific process is as follows:

[0046] Step 1: Add 10g of styrene-divinylbenzene polymer-coated silica gel to 300mL of concentrated hydrochloric acid and water with a volume ratio of 1:1, under electromagnetic stirring, heat and reflux in an oil bath at 90°C for 4h, cool, stand still, and pour out the acid solution, washed several times with water until neutral. After drying, add 70mL of toluene and 25g of aminopropyltriethoxysilane, and react at 105°C for 24h. Add 15mL of trimethylchlorosilane for reaction, the reaction solution is cooled, washed and dried with toluene, diethyl ether and methanol successively, and then a styrene-divinylbenzene polymer-coated silica gel containing aminopropyl groups on the surface is obtained. The number of aminopropyl groups on the surface of silica gel coated with styrene-divinylbenzene polymer is controlled to 0.6 μmol / m by adding the amount of trim...

Embodiment 3

[0051] The preparation of the chiral stationary phase bonded with amylose derivatives, the specific process is as follows:

[0052] Step 1: Add 10g of styrene-divinylbenzene polymer-coated silica gel to 300mL of concentrated hydrochloric acid and water with a volume ratio of 1:1, under electromagnetic stirring, heat and reflux in an oil bath at 90°C for 4h, cool, stand still, and pour out the acid solution, washed several times with water until neutral. After drying, add 70mL of toluene and 0.5g of aminopropyltriethoxysilane, and react at 110°C for 24h. Add 15mL of trimethylchlorosilane for reaction, the reaction solution is cooled, washed and dried with toluene, diethyl ether and methanol successively, and then a styrene-divinylbenzene polymer-coated silica gel containing aminopropyl groups on the surface is obtained. Control the number of aminopropyl groups on the surface of styrene-divinylbenzene polymer coated silica gel by adding the amount of trimethylchlorosilane to 0....

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Abstract

The invention discloses a chiral stationary phase of a bonding amylose derivative and a preparing method thereof. According to the invention, 3,5-dimethyl phenyl carbamate groups are introduced into amylose to obtain the bonding amylose derivative, and then, the bonding amylose derivative is bonded to a solid-phase silica gel carrier coated by a styrene-divinylbenzene polymer through hexamethylene diisocyanate, so that the chiral stationary phase of the bonding amylose derivative is obtained. The chiral stationary phase prepared by the invention is better in selectivity and higher in column efficiency than a chiral compound and can be used under the alkaline condition of pH being 11 for a long time and maintain great effect.

Description

technical field [0001] The invention relates to a high-performance liquid chromatography chiral stationary phase, in particular to a chiral stationary phase bonded with amylose derivatives and a preparation method thereof. Background technique [0002] In recent years, researches on the preparation, synthesis, performance and chiral resolution of racemates of various optically active compounds have been quite active, and have become a hot spot for many researchers and process developers at home and abroad. The direct separation of chiral compounds by HPLC chiral stationary phases (CSPs) has attracted much attention, especially in the research of asymmetric synthesis, asymmetric catalysis and racemic drugs. [0003] Polysaccharide chiral stationary phase is a kind of chiral stationary phase of high performance liquid chromatography, which has wide application, high column efficiency, and good stability. The chiral cavity is suitable for many optical isomers. Following CTA-CS...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B33/00C08G81/00B01J20/26B01J20/30B01J20/29
Inventor 仇伟王明亮肖人杰
Owner NANTONG HONGYU ANALYTICAL INSTR
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