Improved synthesis method of palladium complex

A technology of palladium complexes and synthesis methods, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, compounds of Group 5/15 elements of the periodic table, etc., can solve the problem of multiple synthesis steps and purification Complexity and other problems, to achieve the effect of simple operation method, simple purification and high yield

Inactive Publication Date: 2016-12-21
TIANJIN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] With the deepening of the experiment, the inventors found that there are more synthesis steps and more complicated purification in the preparation method disclosed in 201610352690.6

Method used

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  • Improved synthesis method of palladium complex
  • Improved synthesis method of palladium complex
  • Improved synthesis method of palladium complex

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] PdI 2 (PPh 3 ) 2 The synthetic steps of palladium complex are as follows:

[0023]

[0024] PdCl 2 (PPh 3 ) 2 (50 mg, 0.071 mmol), NaI (107 mg, 0.71 mmol), 10 mL of dichloromethane, and 10 mL of water were added to a 50 mL round-bottom flask successively, and the organic layer was separated after stirring at room temperature for 8 hours, and the Dry over anhydrous sodium sulfate, filter and concentrate, the crude product is recrystallized from dichloromethane / petroleum ether to obtain red crystals which are PdI 2 (PPh 3 ) 2 Complex, yield: 90%. Product NMR and elemental analysis data: 1 H-NMR (400 MHz, CDCl 3 ) δ (ppm):7.71-7.66 (m, 12H, CHar), 7.46-7.37 (m, 18H, CHar); 13 C-NMR (100 MHz, CDCl 3 ) δ(ppm): 135.0, 132.0, 131.2, 128.1.

Embodiment 2

[0026] PdI 2 (PPh 3 ) 2 The synthetic steps of palladium complex are as follows:

[0027]

[0028] PdCl 2 (PPh 3 ) 2 (50 mg, 0.071 mmol), NaBr (74 mg, 0.71 mmol), 10 mL of dichloromethane, and 10 mL of water were successively added to a 50 mL round-bottomed flask, stirred at room temperature for 8 hours, and the organic layer was separated and used Dry over anhydrous sodium sulfate, filter and concentrate, the crude product is recrystallized from dichloromethane / petroleum ether to obtain red crystals which are PdBr 2 (PPh 3 ) 2 Complex, yield: 85%.

[0029] Product NMR and elemental analysis data: 1 H-NMR (400 MHz, CDCl 3 ) δ (ppm): 7.72-7.67 (m,12H, CHar), 7.38-7.34 (m, 18H, CHar); 13 C-NMR (100 MHz, CDCl 3 ) δ (ppm): 135.2, 134.0, 130.2, 127.6.

Embodiment 3

[0031] Catalyst PdBr 2 (PPh 3 ) 2 and PdI 2 (PPh 3 ) 2 The test method and results of the catalytic activity of the Heck coupling reaction are as follows:

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Abstract

The invention discloses an improved synthesis method of a palladium complex (X in a general formula is equal to Br or I) and belongs to the field of organic chemistry. The improved synthesis method is characterized by including: using PdCl2(PPh3)2 and sodium iodide or sodium bromide as raw materials, wherein a feeding molar ratio is 1:10; using dichloromethane and water as solvents according to a volume ratio of 1:1, reacting to obtain a product, and subjecting the product to extracting, washing and filtering to obtain high-quality PdX2(PPh3) palladium complex. The palladium complex is high in yield, the method is simpler, the raw materials are cheaper, and the method has good industrial application prospect.

Description

[0001] This invention was funded by Tianjin Natural Science Foundation (No.16JCYBJC19700). technical field [0002] The invention relates to an improved synthesis method of a palladium complex, belonging to the field of organic chemistry. Background technique [0003] wxya 2 (PPh 3 ) 2 (X=I or Br) palladium complex as an efficient catalyst for Heck coupling reaction has been reported in detail in our previous patent 201610352690.6. [0004] There are not many reports on the synthesis methods of such complexes. For the complexes PdBr 2 (PPh 3 ) 2 , the synthetic methods reported in the literature mainly contain the following: 1) Using tetrakistriphenylphosphorous palladium and 1,2-dibromoethylene as raw materials, THF as solvent ( Gazzetta Chimica Italiana , 1988, 118, 469); 2) with PdCl 2 (CH 3 EN) 2 and lithium bromide as raw materials ( Chemistry-Aeurpoean Journal , 2012, 18, 12803); 3) with PdCl 2 (PPh 3 ) 2 and 4-dimethylaminopyridine hydrobromide as raw ma...

Claims

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Application Information

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IPC IPC(8): C07F9/50B01J31/22
CPCC07F9/5022B01J31/2247B01J2231/4261
Inventor 刘桂艳刘成鑫
Owner TIANJIN NORMAL UNIVERSITY
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