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Multiphase Pd catalyst and preparation method and application thereof

A catalyst and solvent technology, applied in the field of heterogeneous Pd catalyst and its preparation and application, can solve the problems of easily remaining in the product, expensive catalyst, etc., and achieve the effects of small structure influence, simple operation, and mild conditions in the preparation process

Inactive Publication Date: 2010-10-13
EAST CHINA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, the catalyst is expensive and tends to remain in the product, etc.

Method used

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  • Multiphase Pd catalyst and preparation method and application thereof
  • Multiphase Pd catalyst and preparation method and application thereof
  • Multiphase Pd catalyst and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Embodiment 1: the preparation of one of heterogeneous Pd catalyst

[0025] In the first step, the FDU-like ordered mesoporous phenolic resin is FDU-14; in the third step, the metal Pd catalyst is Pd 2 (dba) 3 , the dosage is 4.0g, and one of the heterogeneous Pd catalysts of 51.2g is obtained: [FDU-14-CH 2 PPh 2 / Pd(dba) 2 ].

[0026] The Pd loading of the catalyst was measured by ICP to be 1.8 wt%. The XRD diffraction spectrum and TEM electron microscope photos of the catalyst are shown in figure 1 and figure 2 .

Embodiment 2

[0027] Embodiment 2: the preparation of heterogeneous Pd catalyst two

[0028] In the first step, the FDU-like ordered mesoporous phenolic resin is FDU-14; in the third step, the metal Pd catalyst is Pd 2 (dba) 3 , the dosage is 3.8g, and the second heterogeneous Pd catalyst of 50.8g is obtained: [FDU-14-CH 2 PPh 2 / Pd(dba) 2 ].

[0029]The Pd loading of the catalyst was measured by ICP to be 1.7 wt%. The XRD diffraction pattern and TEM photomicrograph of the catalyst were respectively compared with figure 1 and figure 2 similar.

Embodiment 3

[0030] Embodiment 3: the preparation of heterogeneous Pd catalyst three

[0031] In the first step, the FDU-like ordered mesoporous phenolic resin is FDU-14; in the third step, the metal Pd catalyst is Pd 2 (dba) 3 , the dosage is 3.6g, and the third heterogeneous Pd catalyst of 50.2g is obtained: [FDU-14-CH 2 PPh 2 / Pd(dba) 2 ].

[0032] The Pd loading of the catalyst was measured by ICP to be 1.6 wt%. The XRD diffraction pattern and TEM photomicrograph of the catalyst were respectively compared with figure 1 and figure 2 similar.

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Abstract

The invention relates to a multiphase Pd catalyst and a preparation method and application thereof, belonging to the technical field of catalyst preparation and application. The expressing formula of the catalyst is FDU-CH2PPh2 / PdL2, wherein L denotes dba, OAc or CI, and Pd denotes loading capacity which is 1.5-1.8 weight percent. The preparation method comprises the steps that FDU ordered mesoporous phenolic resin is used as a carrier, a chloride methylene group is introduced through modifying the benzene ring structure of the carrier, the chloride methylene group reacts with monochloro diphenylphosphine to generate a phosphine which takes the FDU ordered mesoporous phenolic resin as a parent substance and finally Pd catalyst is complexed with the phosphine to obtain the multiphase Pd catalyst. The catalyst is particularly suitable for being used as the catalyst in Heck coupling reaction or Suzuki coupling reaction, the catalytic efficiency is high, the catalyst can be recycled for times, and compared with the catalytic activity of the catalyst used at a first time, the catalytic activity of the catalyst used at a sixth time is basically unchanged.

Description

technical field [0001] The present invention relates to a heterogeneous Pd catalyst and its preparation and application. The application refers to the catalyst used as a catalyst in Heck coupling reaction or Suzuki coupling reaction. It has high catalytic efficiency and can be recycled. It belongs to the technology of catalyst and its preparation and application field. Background technique [0002] Pd-catalyzed coupling reaction is an effective method to construct C-C bonds in modern organic synthesis, among which Heck reaction and Suzuki reaction are the most commonly used coupling reactions, widely used in the synthesis of chemicals, agrochemicals and pharmaceutical intermediates and other industrial processes. These coupling reactions are usually carried out in a Pd homogeneous catalytic system under anhydrous conditions, and the reaction yields are high. There are also many review reports on the application of coupling, such as (Miyaura N. and Suzuki A. Chemical Review...

Claims

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Application Information

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IPC IPC(8): B01J31/24B01J37/00C07C69/618C07C67/343C07C57/44C07C51/353C07C255/57C07C253/30C07C15/14C07C1/32C07C43/205C07C41/30C07C255/50
CPCY02P20/584
Inventor 吴海虹姚成福李海岗刘月明吴鹏
Owner EAST CHINA NORMAL UNIVERSITY
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