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The preparation method of 1,1'-di(tert-butylphosphonium)ferrocenepalladium chloride

A technology of tert-butylphosphine and di-tert-butylphosphine, which is applied in the field of preparation of 1,1'-ferrocenepalladium chloride, can solve the problems of low catalyst quality, unfavorable environment and safety, and cumbersome post-treatment. , to achieve broad market prospects and benefits, improve utilization, and simple operation

Active Publication Date: 2022-03-15
JIANGSU SINOCOMPOUND CATALYST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] A. Chloropalladate and DtBPF reaction method, utilize palladium chloride and sodium chloride to react to obtain soluble stronger chloropalladate, and then prepare 1,1'-bis(tert-butylphosphonium)ferrocene chloride Palladium chloride, although this method shortens the reaction time and improves the reaction yield, the post-treatment is cumbersome, and it is easy to introduce K, Na, Li and other heteroions, resulting in low catalyst quality;
[0005] B. Palladium chloride and acetonitrile (benzonitrile) complex compound and DtBPF ligand exchange method, used acetonitrile and benzonitrile are all very toxic chemicals, and the method reaction time is long, and efficient is low; And generally It needs to use a large amount of solvent and needs to be distilled, which is not good for the environment and safety;
[0006] C. Palladium chloride forms a complex with an organic ligand and replaces it with the DtBPF ligand. This method is more costly due to the introduction of other organic ligands, and the reaction time is long and the efficiency is low.

Method used

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  • The preparation method of 1,1'-di(tert-butylphosphonium)ferrocenepalladium chloride
  • The preparation method of 1,1'-di(tert-butylphosphonium)ferrocenepalladium chloride
  • The preparation method of 1,1'-di(tert-butylphosphonium)ferrocenepalladium chloride

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Embodiment 1

[0032] Dissolve palladium and palladium chloride in 20% dilute hydrochloric acid, pass the resulting palladium solution through a D301 anion exchange resin column (Langfang Kaiou), exchange the chloropalladate group on the resin, and 1,1'-bis( Di-tert-butylphosphine) ferrocene (DtBPF) ethanol solution flows through the resin to obtain a red suspension; the suspension is left to stand and then filtered, and the resin is washed with ethanol to separate the resin and the precipitate. Obtain 1,1'-bis(tert-butylphosphino)ferrocene palladium chloride, the productive rate is 82%, the palladium content is 15.48%, the elemental analysis carbon content: 46.74%, nuclear magnetic H-NMR sees attached figure 1 .

Embodiment 2

[0034] Dissolve palladium and palladium chloride in 20% dilute hydrochloric acid, pass the resulting palladium solution through a D301 anion exchange resin column (Langfang Kaiou), exchange the chloropalladate group on the resin, and 1,1'-bis( Di-tert-butylphosphine) ferrocene (DtBPF) solution, the solvent is ethanol and n-hexane, flow through the resin to obtain a red suspension; filter the suspension after standing, and use ethanol to wash the resin to separate the resin and precipitate. Obtain 1,1'-di(tert-butylphosphino)ferrocene palladium chloride, the yield is 87%, the palladium content is 15.38%, the elemental analysis carbon content: 48.09%, nuclear magnetic H-NMR sees attached figure 2 .

Embodiment 3

[0036] Dissolve palladium and palladium chloride in 18% dilute hydrochloric acid, pass the resulting palladium solution through a D301 anion exchange resin column (Langfang Kaiou), exchange the chloropalladate group on the resin, and 1,1'-bis( Di-tert-butylphosphine) ferrocene (DtBPF) tetrahydrofuran ethanol solution flows through the resin to obtain a red suspension; the suspension is left to stand and then filtered, and the resin is washed with ethanol to separate the resin and precipitate. Obtain 1,1'-bis(tert-butylphosphino)ferrocene palladium chloride, the yield is 91%, the palladium content is 15.37%, the elemental analysis carbon content: 47.84%, nuclear magnetic H-NMR sees attached image 3 .

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Abstract

The invention discloses a method for preparing a palladium complex, that is, a method for preparing 1,1'-bis(tert-butylphosphonium)ferrocenepalladium chloride. The method includes: 1. Dissolving palladium metal salt in dilute hydrochloric acid middle; 2. pass the metal liquid through an anion exchange resin column, so that the chloropalladate group is exchanged on the resin; 3. flow the 1,1'-bis(di-tert-butylphosphine) ferrocene (DtBPF) solution through the resin to obtain Red suspension; 4. Filter and wash the precipitate with ethanol to separate the resin and precipitate. The preparation method of the invention is simple to operate, can be produced continuously, has high product purity, can be recycled for use of reaction solution, and has high metal utilization rate.

Description

technical field [0001] The invention relates to the technical field of organic chemistry, in particular to the technical field of preparation of noble metal complex catalysts, in particular to a preparation method of 1,1'-bis(tert-butylphosphino)ferrocenepalladium chloride. Background technique [0002] 1,1'-bis(tert-butylphosphonium)ferrocenepalladium chloride is widely used as a catalyst in the fields of organic chemical industry, pharmaceutical chemical industry and liquid crystal material synthesis. [0003] At present, its main synthesis methods are: [0004] A. Chloropalladate and DtBPF reaction method, utilize palladium chloride and sodium chloride to react to obtain soluble stronger chloropalladate, and then prepare 1,1'-bis(tert-butylphosphonium)ferrocene chloride Palladium chloride, although this method shortens the reaction time and improves the reaction yield, the post-treatment is cumbersome, and it is easy to introduce K, Na, Li and other heteroions, resulting...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F17/02
CPCC07F17/02
Inventor 李娟
Owner JIANGSU SINOCOMPOUND CATALYST