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Preparation method of bis (triphenylphosphine) palladium dichloride

A technology of triphenylphosphine and palladium dichloride, applied in the field of preparation of bis-palladium dichloride, can solve the problems of low synthesis efficiency, long cycle, low yield and the like, and achieves short synthesis cycle, low production cost, and easy operation. simple steps

Inactive Publication Date: 2021-12-07
浙江微通催化新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the invention is to provide a kind of preparation method of two (triphenylphosphine) palladium dichlorides at the deficiencies in the prior art, in order to solve the yield of two (triphenylphosphine) palladium dichlorides in the prior art Low, low purity, low synthesis efficiency and long cycle

Method used

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Examples

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preparation example Construction

[0022] The invention provides a kind of preparation method of bis(triphenylphosphine)palladium dichloride, comprising the following steps:

[0023] 1) Mixing (1,5-cyclooctadiene) palladium dichloride and an organic solvent to obtain a solution 1;

[0024] 2) Mixing triphenylphosphine and an organic solvent to obtain solution 2;

[0025] 3) react after mixing solution 1 and solution 2, and vacuum-dry the reaction product to obtain bis(triphenylphosphine)palladium dichloride.

[0026] The mixing temperature in step 1) of the present invention is preferably 30-70°C, more preferably 40-60°C, more preferably 45-55°C; the mixing time is preferably 15-60min, more preferably 25-50min , more preferably 35-40 min; the mixing is preferably carried out under stirring conditions.

[0027] The mass volume ratio of the (1,5-cyclooctadiene) palladium dichloride and the organic solvent in step 1) of the present invention is preferably 1g: 5-30mL, more preferably 1g: 10-25mL, more preferably ...

Embodiment 1

[0037] Add 10.0g (1,5-cyclooctadiene)palladium dichloride into 80mL tetrahydrofuran under stirring, and dissolve at 55°C for 20min to obtain a homogeneous (1,5-cyclooctadiene)palladium dichloride THF solution.

[0038] Add 25.0 g of triphenylphosphine into 150 mL of tetrahydrofuran under stirring, and dissolve at 55° C. for 20 minutes to obtain a uniform solution of triphenylphosphine in tetrahydrofuran.

[0039] Under rapid stirring conditions, (1,5-cyclooctadiene)palladium dichloride tetrahydrofuran solution was added dropwise to triphenylphosphine tetrahydrofuran solution at a rate of 30mL / min, and the reaction was stirred at 55°C 0.5h. The reaction product was cooled, filtered, washed, and drained, and the obtained filter cake was vacuum-dried at 60°C and -0.05MPa vacuum for 3.5 hours to obtain the target product bis(triphenylphosphine)palladium dichloride.

[0040] The quality of the bis(triphenylphosphine)palladium dichloride of Example 1 is 24.53g, the product yield i...

Embodiment 2

[0042] Add 10.0g (1,5-cyclooctadiene) palladium dichloride into 100mL dichloromethane under stirring state, and dissolve at 40°C for 40min to obtain uniform (1,5-cyclooctadiene) dichloride Palladium in dichloromethane solution.

[0043] Add 30.0 g of triphenylphosphine into 600 mL of absolute ethanol under stirring, and dissolve at 40° C. for 45 minutes to obtain a uniform ethanol solution of triphenylphosphine.

[0044] Under rapid stirring conditions, the dichloromethane solution of (1,5-cyclooctadiene)palladium dichloride was added dropwise to the ethanol solution of triphenylphosphine at a rate of 50mL / min. The reaction was stirred for 3h. The reaction product was cooled, filtered, washed, and drained, and the obtained filter cake was vacuum-dried at 70°C and -0.06 MPa for 5.5 hours to obtain the target product bis(triphenylphosphine)palladium dichloride.

[0045]The quality of the bis(triphenylphosphine)palladium dichloride of Example 2 is 24.46g, the product yield is 9...

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Abstract

The invention belongs to the technical field of palladium catalysts. The invention provides a preparation method of bis (triphenylphosphine) palladium dichloride, which comprises the steps of mixing (1, 5-cyclooctadiene) palladium dichloride and an organic solvent to obtain a solution 1; mixing triphenylphosphine with an organic solvent to obtain a solution 2; and mixing the solution 1 and the solution 2, reacting, and carrying out vacuum drying on a reaction product to obtain bis (triphenylphosphine) palladium dichloride. According to the preparation method, the content of heteroions in the product and the requirement for reaction conditions are reduced, dangerous chemicals are not involved in the whole reaction process, the reaction conditions are mild, and the operation environment is better and safer. The preparation method is low in production cost, short in synthesis period, high in efficiency and simple in operation step, the yield of the target product bis (triphenylphosphine) palladium dichloride is greater than or equal to 99.2%, and the purity of the target product bis (triphenylphosphine) palladium dichloride is greater than or equal to 98.5%.

Description

technical field [0001] The invention relates to the technical field of palladium catalysts, in particular to a preparation method of bis(triphenylphosphine)palladium dichloride. Background technique [0002] Bis(triphenylphosphine)palladium dichloride is an important palladium catalyst in chemical reactions, and is widely used in organic catalysis and pharmaceutical and chemical industries. For example, bis(triphenylphosphine)palladium dichloride is an efficient catalyst for coupling reactions such as Sonogoshira coupling, carbonylation of halides, aldehydes from haloalkanes, carboxylic acids, and amides. [0003] At present, the main synthesis methods of bis(triphenylphosphine)palladium dichloride include: 1) direct reaction method of palladium chloride and triphenylphosphine; 2) complex compound of palladium chloride and acetonitrile (or benzonitrile) and Triphenylphosphine ligand exchange method; 3) tetrachloropalladate (potassium salt, sodium salt) and triphenylphosphin...

Claims

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Application Information

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IPC IPC(8): C07F15/00
CPCC07F15/0066
Inventor 黄鹏陈华刘斌杨立强谢智平魏青王惟施春苗
Owner 浙江微通催化新材料有限公司
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