Preparation method of tri (dibenzylideneacetone) dipalladium complex

A technology of dibenzylideneacetone and complexes, which is applied in the directions of palladium organic compounds, platinum group organic compounds, chemical instruments and methods, etc., can solve the problems of affecting product quality, affecting catalytic activity, low yield and the like, and shortening the production time. time, improving utilization rate, and the effect of high product purity

Active Publication Date: 2020-07-31
JIANGSU SINOCOMPOUND CATALYST
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  • Application Information

AI Technical Summary

Problems solved by technology

But the complex that this method obtains is usually not high-purity tris(dibenzylideneacetone) dipalladium (0), but the mixture of several complexes, low-purity complexes not only affect the catalytic activity, but also affect the product quality
[0003] However, because the price of palladium is extremely expensive, and there are no natural resources of palladium in China, the production cost of tris(dibenzylideneacetone)dipalladium(0) is low and the production cost remains high at present

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Dissolve palladium acetate in dichloromethane; dissolve dibenzylidene acetone in absolute ethanol and toluene (1:1); fill the two-stage 5L reactor with self-made redox resin; The solution and the dibenzylidene acetone solution are added in proportion and passed through the two-stage reactor at 5ml / min; the product is condensed and crystallized with condensed water, and the liquid is transferred to the previous step for the next reaction. The elemental analysis of the obtained product is C: 66.72%, H: 4.71%; Pd, the content is 23.36%, the product purity is more than 99%, and the primary yield is 89%.

Embodiment 2

[0020] Dissolve palladium sulfate in dichloromethane; dissolve dibenzylidene acetone in the reaction solution of Example 1; fill it into a two-stage 5L reactor with self-made redox resin; The benzyl acetone solution is added in proportion and passed through the two-stage reactor at 5ml / min; the product is condensed and crystallized with condensed water, and the liquid is transferred to the previous step for the next reaction. The elemental analysis of the product obtained is C: 66.37%, H: 4.60%, Pd, the content is 23.06%, the product purity is more than 99%, and the primary yield is 90%.

Embodiment 3

[0022] Dissolve palladium chloride in dichloromethane; dissolve dibenzylideneacetone in N,N-dimethylformamide and toluene (1:1); use self-made redox resin to fill into two-stage 50L reactor ; At 80°C, add the palladium solution and the dibenzylidene acetone solution in proportion to pass through the two-stage reactor at 150ml / min; the product uses condensed water for condensation and crystallization, and the liquid is transferred to the previous step for the next reaction. The elemental analysis of the obtained product is C: 67.36%, H: 5.06%, Pd, the content is 23.67%, the product purity is more than 99%, and the yield is 88%.

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Abstract

The invention discloses a preparation method of a palladium complex tri (dibenzylideneacetone) dipalladium (0). The preparation method comprises the following steps: dissolving palladium metal salt inpure water; dissolving dibenzylidene acetone in a proper solvent; filling the reactor with redox resin; adding the palladium metal salt solution and the dibenzylidene acetone solution into the reactor in proportion at a proper speed at a certain temperature; and finally, pumping the reactor solution into a condenser for solid-liquid separation to obtain the palladium complex tri (dibenzylideneacetone) dipalladium (0).

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 method for preparing palladium complex tris(dibenzylideneacetone)dipalladium(0). Background technique [0002] Regarding the palladium(0) complex Pd(dba), it is usually prepared by adding sodium acetate and excess dba to a hot solution of sodium chloropalladate in methanol or a hot solution of palladium chloride in methanol. The solution was cooled with stirring, whereby the complex was precipitated. The complex was then collected by filtration and washed with water and then with acetone. But the complex that this method obtains is usually not high-purity tris(dibenzylideneacetone) dipalladium (0), but the mixture of several complexes, low-purity complexes not only affect the catalytic activity, but also affect the product quality. [0003] However, because the price of palladium ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00
CPCC07F15/006
Inventor 李娟
Owner JIANGSU SINOCOMPOUND CATALYST
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