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Silica gel bonded with single-chiral spiral polyether, preparation method thereof, and application thereof used as chiral immobile phase of high-performance liquid chromatographic column

A bonding and helical technology, which is applied in the field of silica gel bonded with monochiral helical polyether and its preparation and use as a chiral stationary phase in high performance liquid chromatography, which can solve problems such as application limitations

Inactive Publication Date: 2011-10-12
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the degree of polymerization of this polymer is only about 7-9, which is very limited in application.

Method used

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  • Silica gel bonded with single-chiral spiral polyether, preparation method thereof, and application thereof used as chiral immobile phase of high-performance liquid chromatographic column
  • Silica gel bonded with single-chiral spiral polyether, preparation method thereof, and application thereof used as chiral immobile phase of high-performance liquid chromatographic column
  • Silica gel bonded with single-chiral spiral polyether, preparation method thereof, and application thereof used as chiral immobile phase of high-performance liquid chromatographic column

Examples

Experimental program
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Effect test

example 1

[0056] Example 1: Activation of silica gel

[0057] Put 60g of spherical silica gel into a 2000mL three-necked bottle, add 1500mL of 10% hydrochloric acid, and heat to reflux for 10h. Filter after cooling. The filter cake was washed with distilled water until the washed water was neutral, and then washed several times with acetone. After the acetone on the surface was volatilized, the filter cake was dried in an oven at 160°C for 8 hours, and then stored in a desiccator to cool for later use.

example 2

[0058] Example 2: Preparation of silica gel bonded with monochiral helical polyether having poly[(S)-3-(9-methylfluoren-9-yl)-1,2-propylene oxide] skeleton structure. method one.

[0059] Add 8 mmoles of (S)-3-(9-methylfluoren-9-yl)-1,2-propylene oxide and 0.020 g of KOH into a reaction flask equipped with a magnetic stirring bar. The reaction bottle was vacuumized and filled with high-purity argon, and the operation of pumping and filling with argon was repeated twice. Place the reaction bottle in an oil bath at 100-110°C, and react under magnetic stirring. When the reactant was solidified and the stirring bar could not be stirred, the temperature of the oil bath was lowered to 80°C, and 3 mL of anhydrous toluene was added with a syringe. After the solid block was completely dissolved, 0.4 mmol (0.095 g) of 3-glycidylpropyltrimethoxysilane was added, and the mixture was stirred and reacted in an oil bath at 80° C. for 4 hours. Then, the reaction solution was taken out with...

example 3

[0060] Example 3: Preparation of silica gel bonded with monochiral helical polyether having poly[(S)-3-(9-ethylfluoren-9-yl)-1,2-propylene oxide] skeleton structure. Method Two.

[0061] Add 8 mmoles of (S)-3-(9-ethylfluoren-9-yl)-1,2-propylene oxide into a reaction flask equipped with a magnetic stirring bar. The reaction bottle was vacuumized and filled with high-purity argon, and the operation of pumping and filling with argon was repeated twice. Inject 3 mL of anhydrous toluene and 0.2 mmol of potassium tert-butoxide in THF with a syringe. The reaction bottle was placed in an oil bath at 100-110° C., and reacted for 12 hours under magnetic stirring. The temperature of the oil bath was lowered to 80° C., 0.4 mmol (0.095 g) of 3-glycidylpropyltrimethoxysilane was added, and the mixture was stirred and reacted in an oil bath of 80° C. for 4 hours. Then, the reaction solution was taken out with a syringe, quickly injected into a three-necked bottle containing 60 mL of anhyd...

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Abstract

The invention discloses silica gel bonded with a single-chiral spiral polyether which has a frame structure of poly[3-(9-alkylfluoren-9-yl)-1,2-epoxy propane], a preparation method thereof, and application thereof used as a chiral immobile phase of a high-performance liquid chromatographic column. The invention has the following technical effects that: the silica gel bonded with a single-chiral spiral polyether which has the frame structure of poly[3-(9-alkylfluoren-9-yl)-1,2-epoxy propane] is used as the chiral immobile phase of the high-performance liquid chromatographic column, which can separate and analyze a plurality of racemes such as alcohols, ketones, esters, carboxylic acids and amines.

Description

technical field [0001] The present invention relates to the preparation of silica gel of monochiral helical polyether bonded with poly[3-(9-hydrocarbylfluoren-9-yl)-1,2-propylene oxide] skeleton structure and its use in high performance liquid chromatography Chiral stationary phases for the analysis and separation of racemates. Background technique [0002] In 1979, Okamoto used the helical selective polymerization method to polymerize trityl methacrylate, and obtained polytrityl methacrylate (J.Am.Chem.Soc. 1979, 101, 4763). Then Okamoto found that this monochiral helical polytrityl methacrylate can be used as a high-performance liquid chromatography (HPLC) chiral stationary phase to separate racemates (J.Am.Chem.Soc.1980 , 102, 6358; J. Am. Chem. Soc., 1981, 103, 6971). Now the chiral stationary phase has been successfully made into commercial HPLC chiral chromatography columns. [0003] Although the monochiral helical polytrityl methacrylate as the chiral stationary p...

Claims

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Application Information

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IPC IPC(8): C08G65/338C08G65/336C08G65/06B01J20/29G01N30/36
Inventor 阳年发刘德贤张劲杨利文
Owner XIANGTAN UNIV
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