Preparation method and application of cross-linking type polymerization catalyst

A polymerization catalyst and cross-linking technology, which is applied in the field of preparation of cross-linking polymerization catalysts, can solve problems such as non-recycling and recycling, low catalyst loading capacity, and easy deactivation of catalysts, and achieve easy operation and easy post-processing , the effect of expanding the scope of application

Inactive Publication Date: 2016-02-24
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The heterogeneous solid-supported catalysts in the prior art have low immobilization capacity, low yield, easy deactivation of the catalyst, l

Method used

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  • Preparation method and application of cross-linking type polymerization catalyst
  • Preparation method and application of cross-linking type polymerization catalyst
  • Preparation method and application of cross-linking type polymerization catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The first step: Weigh 2.04g p-vinylbenzoic acid and 0.52g 4-dimethylaminopyridine (DMAP) in 20ml dichloromethane, and then add 6.6g 1-(3-dimethylaminopropyl)-3-in three times Ethylcarbodiimide hydrochloride (EDCI), every 15 minutes, add 5.36g quinidine (Cinchonidine) solid at the end, carry out the esterification reaction at room temperature for 12h, spin off the solvent after the reaction, add 20ml Dichloromethane and an equal volume of distilled water, the separated aqueous phase was extracted twice with 40ml of dichloromethane, and the organic phases were combined and extracted once with 30ml of saturated brine. The extracted organic phase was dried with anhydrous sodium sulfate After filtration, concentration and silica gel column chromatography (EA:PE=1:5), a pale yellow oily compound was obtained as a catalyst precursor, and the yield was 86%.

[0016] Step 2: Weigh 0.91g of the catalyst precursor prepared above, mix 0.52g divinylbenzene and 0.043g azobisisobutyronit...

Embodiment 2

[0018] Weigh 0.015g (5mol%) of the catalyst prepared above, 0.076g β-ketoester (methyl1-oxo-2,3-dihydro-1H-indene-2-carboxylate) and 0.034g sodium bicarbonate dissolved in 4ml ethyl acetate After stirring for 10 minutes at -40°C, 0.150g of chlorinated reagent (5,7,7-trichloroquinolin-8(7H)-one) was added to carry out the asymmetric α-chlorination catalytic reaction of the following reaction structure:

[0019]

[0020] After the reaction, the catalyst was filtered out, and 10ml of distilled water was added. The separated aqueous phase was extracted twice with an equal volume of ether, and the organic phases were combined and extracted once with saturated brine. The extracted organic phase was dried, filtered, concentrated and silica gel The product obtained by column chromatography was α-chloroβ-ketoester, and its enantioselectivity was measured by high performance liquid chromatography.

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Abstract

The invention discloses a preparation method and application of a cross-linking type polymerization catalyst. The preparation method is characterized by including performing a synthesis reaction to form an intermediate compound of which molecule contains vinyl benzene by using cinchona alkaloid and derivative of vinyl benzene, and performing a polymerization reaction of the intermediate compound and the cross-linking agent divinyl benzene to form a polymer catalyst in the presence of an initiator. The catalyst is used for an asymmetric alpha-chlorination catalytic reaction of beta-ketonic ester and chlorinated reagent, has high catalytic activity, is easy to separate, and can be recycled. Compared with the prior art, the preparation method has simple preparation, easy operation, easy post-treatment, high raw material utilization ratio, optimized reaction condition and reduced reaction requirement, especially is used for the compound obtained by constructing a chiral center on the different carbon of beta-ketonic ester, and has an important practical significance of researching medicinal chemistry and medical intermediate compound.

Description

Technical field [0001] The invention relates to the technical field of catalysts and organic catalysis applications, in particular to a preparation method and application of a crosslinked polymerization catalyst. Background technique [0002] Since cinchona was used by researchers in organocatalytic reactions, such small organic molecules have been developed and used in different types of reactions. From the perspective of the type of catalyst, it can be divided into homogeneous catalysts and heterogeneous catalysts. Most heterogeneous catalysts are effective homogeneous catalysts supported on solid materials, such as SBA-15, FDU and other mesoporous or other materials. However, the solid loading of the catalyst is always limited, and the catalytic performance of the catalyst cannot be completely maintained. Changing the solid loading type of the catalyst is also a way to optimize the reaction. Compared with traditional homogeneous catalysts, heterogeneous catalysts may not be ...

Claims

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Application Information

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IPC IPC(8): C08F212/36C08F226/06B01J31/06C07C69/757C07C67/307
CPCB01J31/06B01J2231/4277C07C67/307C07C69/757C08F226/06C08F212/36
Inventor 吴海虹刘廷英吴鹏
Owner EAST CHINA NORMAL UNIV
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