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A kind of preparation method of three (dibenzylideneacetone) dipalladium (0)

A technology of dibenzylideneacetone and palladium dichloride is applied in chemical instruments and methods, compounds containing elements of Group 8/9/10/18 of the periodic table, palladium organic compounds, etc. The problems such as the amount of added dibenzylideneacetone, long reaction time, and difficult operation are solved, and the effects of short reaction time, simple preparation method and simple equipment are achieved.

Active Publication Date: 2021-12-21
XIAN CATALYST NEW MATERIALS CO LTD
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  • Abstract
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  • Claims
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Problems solved by technology

Document J.C.S.Dzlton, 1974,169 mentions the method that adopts dibenzylidene acetone, sodium acetate, sodium chloropalladate to react and synthesize two (dibenzylidene acetone) palladium (0) at low temperature, adopts methanol solvent at low temperature The reaction time is long and the equipment is complicated; it needs to be reacted under anhydrous and oxygen-free conditions, and the operation is difficult; and the addition of the ligand dibenzylidene acetone is not strictly controlled, and the obtained product is a mixture
Patent CN 102010445 A has reported the method that adopts dibenzylidene acetone, sodium acetate, palladium dichloride to react and synthesize bis(dibenzylidene acetone) palladium (0) in dehydrated alcohol, and it has only reported bis(dibenzylidene acetone) palladium (0) Synthetic method of benzylacetone) palladium (0), not involving the synthesis research of tris (dibenzylideneacetone) dipalladium (0)

Method used

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  • A kind of preparation method of three (dibenzylideneacetone) dipalladium (0)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 1.1 Preparation of palladium dichloride:

[0021] Add nitric acid with a mass concentration of 65% to high-purity palladium powder with a mass purity of not less than 99.95%. The quality of nitric acid is 0.7 times that of the palladium powder. After heating and waiting for its reaction, slowly add hydrochloric acid with a mass concentration of 36%. It is 2.1 times the mass of palladium powder. After the palladium powder is completely dissolved, a small amount of hydrochloric acid with a mass concentration of 36% is added several times to completely replace the nitric acid in the solution. If the particle size is less than 10 μm, palladium dichloride with the desired mass purity of 99.9% can be obtained.

[0022] 1.2 Synthesis of dibenzylideneacetone:

[0023] Measure 10L mass concentration of 10% sodium hydroxide solution and 8L mass concentration of 95% absolute ethanol in a 30L glass reactor, add 10.5L benzaldehyde and 0.36L acetone successively under mechanical sti...

Embodiment 2

[0025] Preparation of tris(dibenzylideneacetone)dipalladium(0):

[0026] Step 1. Under a nitrogen atmosphere, add 32 L of absolute ethanol and 0.85 kg of anhydrous sodium acetate into a glass reactor heated by a water bath. When the system temperature is heated to 80° C., add 3 kg of dibenzylidene acetone obtained in Example 1, and stir After reacting for 20 minutes, add ice to the water-bath heater to cool the system down to 45°C rapidly, then add 1kg of palladium dichloride prepared in Example 1, react at 45°C for 3h, and filter through a funnel to obtain bis(dibenzylideneacetone ) Palladium(0);

[0027] Step 2. Under a nitrogen atmosphere, add 5 L of acetone to a glass reactor heated by a water bath. After the temperature of the acetone in the reactor is heated to 30° C., add bis(dibenzylideneacetone) palladium (0) obtained in Step 1, 30 React at ℃ for 3 hours, filter, wash with deionized water and absolute ethanol, and dry in an oven at 40℃ to obtain the product tris(dibe...

Embodiment 3

[0030] Preparation of tris(dibenzylideneacetone)dipalladium(0):

[0031] Step 1. Under a nitrogen atmosphere, add 18 L of absolute ethanol and 0.48 kg of anhydrous sodium acetate into a glass reactor heated by a water bath, and add 0.86 kg of dibenzylidene acetone obtained in Example 1 when the system temperature is heated to 60° C. After stirring and reacting for 40 minutes, add ice to the water bath heater to rapidly cool the system to 57° C., then add 0.42 kg of palladium dichloride prepared in Example 1, react for 1.5 hours at 57° C., and filter through a funnel to obtain bis(dimethoxymide) benzylacetone) palladium (0);

[0032] Step 2. Under a nitrogen atmosphere, add 2.5 L of acetone to a glass reactor heated by a water bath. After the temperature of the acetone in the reactor is heated to 15° C., add bis(dibenzylideneacetone) palladium (0) obtained in Step 1, Heat the reaction for 1 h, filter, wash with deionized water and absolute ethanol, and dry in an oven at 30°C t...

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Abstract

The invention discloses a preparation method of tris(dibenzylideneacetone)dipalladium(0). The method comprises: 1. Under a nitrogen atmosphere, the ligand dibenzylideneacetone, palladium dichloride and anhydrous Sodium acetate is added in the dehydrated alcohol of stirring state and heated reaction, obtains solid bis (dibenzylidene acetone) palladium (0) after filtration; Two, under nitrogen atmosphere, the solid bis (dibenzylidene acetone) that obtains in step Acetone)palladium(0) was added into acetone in a stirring state for reaction, the retentate was washed after filtration, and the washed retentate was dried to obtain tris(dibenzylideneacetone)dipalladium(0). The present invention adopts dehydrated alcohol, dibenzylidene acetone, palladium dichloride and anhydrous sodium acetate to first prepare bis(dibenzylidene acetone) palladium (0), and then obtains tris(dibenzylidene acetone) through acetone solution treatment ) dipalladium (0), the three (dibenzylideneacetone) dipalladium (0) obtained has higher purity.

Description

technical field [0001] The invention belongs to the technical field of preparation of zero-valent palladium catalysts, and in particular relates to a preparation method of tris(dibenzylideneacetone)dipalladium(0). Background technique [0002] Tris(dibenzylideneacetone)dipalladium(0) is an important zero-valent palladium catalyst, which is widely used in coupling, hydrogenation, carbonylation and other reactions in organic synthesis. Used in combination with different ligands, the zero-valent palladium active species with high catalytic activity can be formed in situ, and it has been widely used in carbon-carbon bond and carbon-heteroatom bond formation reactions. It has high catalytic activity in the coupling reaction of chlorinated aromatic hydrocarbons and phenylboronic acid. It can also be used for the Stille coupling of chlorinated arenes and organotin, the Heck cross-coupling reaction of chlorinated arenes and alkenes, and the asymmetric Heck arylation reaction of int...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F15/00
CPCC07F15/006
Inventor 张洁兰陈丹颜攀墩校大伟李岳锋万克柔
Owner XIAN CATALYST NEW MATERIALS CO LTD
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