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In situ supported catalyst and preparation method and application thereof

A supported catalyst and catalyst technology, applied in the direction of organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve a large number of carriers, catalyst removal, low loading, etc question

Inactive Publication Date: 2014-03-12
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this kind of method requires a large amount of carrier, the loading amount is small, the catalyst is easy to be removed from the carrier, and the recycling effect is not good.

Method used

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  • In situ supported catalyst and preparation method and application thereof

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Effect test

Embodiment 1

[0008] Embodiment 1: in-situ supported catalyst 1

[0009] At room temperature, zinc oxide, 2-methylimidazolium, and palladium ions were reacted by mechanochemical method for 30 minutes (MM40030HZ / min) at a material ratio of 1:2:0.001, and then hydroborated in an ice bath. sodium reduction, deionized water, ethanol washing, vacuum drying to obtain the in-situ supported catalyst.

Embodiment 2

[0010] Embodiment 2: in-situ supported catalyst 2

[0011] At room temperature, zinc oxide, 2-methylimidazolium and palladium ions were reacted by mechanochemical method for 30 minutes (MM40030HZ / min) at a mass ratio of 1:2:0.01, and then hydroborated in an ice bath. sodium reduction, deionized water, ethanol washing, vacuum drying to obtain the in-situ supported catalyst.

[0012] Example 2: Suzuki reaction catalyzed by in-situ supported catalysts

[0013] Add in-situ supported catalyst Pd / ZIF-8, bromobenzene (and its derivatives), phenylboronic acid (and its derivatives) to the reaction system in sequence, the ratio of the amount of the three substances is 0.005:1:2, Solvent Mixed solvent of deionized water and ethanol, reaction temperature 80°C, after 6 hours of reaction, filter, catalyst washed with deionized water and ethanol, vacuum dried, recycled; liquid phase part extracted with ethyl acetate, dried over anhydrous sodium sulfate, The corresponding Suzuki reaction pr...

Embodiment 3

[0014] Example 3: Suzuki reaction catalyzed by in-situ supported catalysts

[0015] Add in-situ supported catalyst Pd / ZIF-8, bromobenzene (and its derivatives), phenylboronic acid (and its derivatives) to the reaction system in sequence, the ratio of the amount of the three substances is 0.001:1:2, Solvent Mixed solvent of deionized water and ethanol, reaction temperature 80°C, after 6 hours of reaction, filter, catalyst washed with deionized water and ethanol, vacuum dried, recycled; liquid phase part extracted with ethyl acetate, dried over anhydrous sodium sulfate, The corresponding Suzuki reaction products were separated by column chromatography.

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Abstract

The invention discloses an in situ supported catalyst and a preparation method thereof. The catalyst is used for catalyzing Suzuki reaction. The in site supported catalyst comprises zinc oxide, 2-methylimidazole and palladium ion and is prepared through a mechanochemical method. The catalyst is simple to prepare, can be used for catalyzing bromobenzene (and derivatives thereof) and borophenylic acid (and derivatives thereof) with high activity and high selectivity to perform Suzuki reaction, can be separated from the product simply, and can be reused for times.

Description

technical field [0001] The invention belongs to the technical field of Suzuki reaction catalysts, and in particular relates to a preparation method of an in-situ supported catalyst and an application of catalytic Suzuki reactions. Background technique [0002] In the palladium-catalyzed Suzuki coupling reaction, biphenyls (and their derivatives) constructed from halogenated aromatic hydrocarbons and arylboronic acids are important organic synthesis intermediates and are widely used in petrochemical, fine chemical and organic synthesis fields. However, homogeneous catalysts are difficult to separate, easy to decompose, and cannot be recycled, which limits their wide application. For this reason, people try to overcome the above-mentioned shortcomings by heterogeneous homogeneous catalysts. At present, such catalysts are generally supported on organic polymers or inorganic supports. But this kind of method needs a large amount of carrier, the loading amount is small, the cat...

Claims

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Application Information

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IPC IPC(8): B01J31/28C07C15/14C07C1/32
Inventor 马涛曹荣黄远标
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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