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Preparation method of 1,1'-bis (tert-butylphosphine) ferrocene palladium 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 unfavorable environment and safety, low catalyst quality, long reaction time, etc. , to achieve broad market prospects and benefits, low cost, simple operation

Active Publication Date: 2020-06-16
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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  • Preparation method of 1,1'-bis (tert-butylphosphine) ferrocene palladium 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 preparation method of a palladium complex, namely a preparation method of 1,1'-bis(tert-butylphosphine)ferrocene palladium chloride, which comprises the following steps: 1. dissolving palladium metal salt in diluted hydrochloric acid; 2, enabling the metal solution to pass through an anion exchange resin column to enable chloropalladate radicals to be exchanged on resin;3, enabling the 1,1'-bis(di-tert-butylphosphine)ferrocene (DtBPF) solution to flow through the resin to obtain red turbid liquid; and 4, filtering, and washing the precipitate with ethanol to separatethe resin and the precipitate. The preparation method disclosed by the invention is simple to operate, capable of realizing continuous production, high in product purity, recyclable in reaction liquid and high in 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 synthetic 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 Applications(China)
IPC IPC(8): C07F17/02
CPCC07F17/02
Inventor 李娟
Owner JIANGSU SINOCOMPOUND CATALYST
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