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Crystal structure of ester Pd-NHC molecular complex and synthetic method

A synthesis method and complex technology, which are used in the preparation of organic compounds, organic compound/hydride/coordination complex catalysts, organic chemistry methods, etc. Electronic structure and other issues, to achieve the effect of good catalytic activity and excellent catalytic performance

Inactive Publication Date: 2019-01-18
LIAOCHENG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] (1) In the prior art, the Pd-NHC molecular complexes modified by organic functional groups do not have better catalytic activity, and the Pd-NHC molecular complexes in the prior art do not have the electronic structure to regulate the NHC molecular ligands
[0007] (2) In the prior art, it is not possible to use cheap chlorides to provide a low-cost, high-efficiency catalytic performance ester Pd-NHC molecular complex

Method used

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  • Crystal structure of ester Pd-NHC molecular complex and synthetic method
  • Crystal structure of ester Pd-NHC molecular complex and synthetic method
  • Crystal structure of ester Pd-NHC molecular complex and synthetic method

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preparation example Construction

[0047] Such as figure 1 As shown, the synthesis method of the ester Pd-NHC molecular complex provided by the embodiment of the present invention specifically includes the following steps:

[0048] S101: In nitrogen atmosphere or air, carboxylate ligand, divalent palladium ion metal salt (0.05-1.0mmol), chloride, pyridine and pyridine derivative solvent are placed in a conventional airtight container, and heated for 10-2000 minutes;

[0049] S102: cooling to room temperature, evaporating the solvent in vacuo to obtain a solid residue;

[0050]S103: dissolving the obtained solid residue in a mixed solvent of dichloromethane and water, and separating through a separatory funnel to obtain an organic phase;

[0051] S104: washing the obtained organic phase with 5% copper sulfate solution and saturated brine, drying with anhydrous sodium sulfate, and evaporating the solvent in vacuo to obtain a solid residue;

[0052] S105: Recrystallize the obtained solid residue in a mixed solv...

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Abstract

The invention belongs to the technical field of catalysts, and discloses an ester Pd-NHC molecular complex and a synthetic method. The synthetic method comprises the steps that in a nitrogen atmosphere or air, a carboxylic ester ligand, divalent palladium ion metal salt, chloride, pyridine and a pyridine derivative solvent are placed in a conventional closed container and are heated for 10-2000 minutes; cooling is carried out to reach the room temperature, and vacuum evaporation is carried out on the solvent so as to obtain solid residues; the obtained solid residues are dissolved in a mixed solvent of dichloromethane and water, and separation is carried out through a separating funnel so as to obtain an organic phase; the organic phase is washed by using a 5% copper sulfate solution and saturated salt water and is dried by using anhydrous sodium sulfate, and vacuum evaporation is carried out on a solvent so as to obtain solid residues; and the obtained solid residues are recrystallized in a mixed solvent of chloroform and normal hexane so as to obtain Pd-NHC molecular crystals. According to the ester Pd-NHC molecular complex and the synthetic method, the carboxylic ester functional group modified Pd-NHC molecular complex is synthesized and a crystal structure of the Pd-NHC molecular complex is obtained.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to a crystal structure and a synthesis method of an ester Pd-NHC molecular complex. Background technique [0002] At present, the existing technologies commonly used in the industry are as follows: [0003] Pd-NHC molecular complexes are an important class of organometallic catalysts, which not only have excellent catalytic performance, but also can exist stably in humid air. Typical representatives of such Pd-NHC molecular complexes are PEPPSI type catalysts (C. Valent et al, Angew. Chem. Int. Ed. 2012, 51, 3314–3332). In the molecular structure of PEPPSI-type catalysts, the organoalkane functional group can significantly regulate its catalytic activity through the steric hindrance effect. However, this type of catalyst is a homogeneous catalyst. The catalytic reaction requires the use of volatile and highly toxic organic solvents. It is difficult to separate the ca...

Claims

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Application Information

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IPC IPC(8): C07F15/00B01J31/22C07C67/343C07C69/76
CPCB01J31/2269C07B2200/13C07C67/343C07F15/006C07C69/76
Inventor 姚清侠周杨段文增霍艳敏王敏
Owner LIAOCHENG UNIV
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