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Synthetic method of [1,1'- bis-(diphenyl phosphine) ferrocene] palladium dichloride methylene dichloride complex

A technology of diphenylphosphine and dichloromethane, applied in the field of chemical synthesis, can solve the problems of complicated preparation process and high production cost, and achieve the effects of simple reaction process, low production cost and mild reaction conditions

Active Publication Date: 2012-07-25
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The preparation process of this approach is more loaded down with trivial details, and the production cost is higher

Method used

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  • Synthetic method of [1,1'- bis-(diphenyl phosphine) ferrocene] palladium dichloride methylene dichloride complex
  • Synthetic method of [1,1'- bis-(diphenyl phosphine) ferrocene] palladium dichloride methylene dichloride complex

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Step 1, dissolving 2.00 grams of sodium chloropalladate in 30 mL of absolute ethanol to obtain an ethanol solution of sodium chloropalladate;

[0018] Step 2, 4.15 grams of 1,1'-bis(diphenylphosphino)ferrocene was dissolved in 41mL of dichloromethane to obtain a dichloromethane solution of 1,1'-bis(diphenylphosphino)ferrocene ;

[0019] Step 3. Add the ethanol solution of sodium chloropalladate described in step 1 dropwise to the dichloromethane solution of 1,1'-bis(diphenylphosphino)ferrocene described in step 2 under stirring condition , stirred and reacted for 1 h at a temperature of 25°C, filtered the reaction solution after the reaction, and obtained 5.01 grams of orange-red [1,1'-bis(diphenylphosphino)ferrocene]dichloropalladium dichloromethane complex The compound crystallized with a yield of 90.46%.

[0020] In this embodiment, dichloromethane is directly used as a solvent, and the target product [1,1'-bis(diphenylphosphino)ferrocene]dichloropalladium dichloro...

Embodiment 2

[0023] Step 1, dissolving 2.00 grams of sodium chloropalladate in 40 mL of absolute ethanol to obtain an ethanol solution of sodium chloropalladate;

[0024] Step 2, 4.52 grams of 1,1'-bis(diphenylphosphino)ferrocene was dissolved in 45mL of dichloromethane to obtain a dichloromethane solution of 1,1'-bis(diphenylphosphino)ferrocene ;

[0025] Step 3. Add the ethanol solution of sodium chloropalladate described in step 1 dropwise to the dichloromethane solution of 1,1'-bis(diphenylphosphino)ferrocene described in step 2 under stirring condition , stirred and reacted for 1 h at a temperature of 25°C, filtered the reaction solution after the reaction, and obtained 5.02 g of orange-red [1,1'-bis(diphenylphosphino)ferrocene]dichloropalladium dichloromethane complex The compound crystallized with a yield of 90.64%.

[0026] In this embodiment, dichloromethane is directly used as a solvent, and the target product [1,1'-bis(diphenylphosphino)ferrocene]dichloropalladium dichlorometh...

Embodiment 3

[0028] Step 1, dissolving 2.00 grams of sodium chloropalladate in 20 mL of absolute ethanol to obtain an ethanol solution of sodium chloropalladate;

[0029] Step 2, 4.15 grams of 1,1'-bis(diphenylphosphino)ferrocene was dissolved in 21mL of dichloromethane to obtain a dichloromethane solution of 1,1'-bis(diphenylphosphino)ferrocene ;

[0030] Step 3. Add the ethanol solution of sodium chloropalladate described in step 1 dropwise to the dichloromethane solution of 1,1'-bis(diphenylphosphino)ferrocene described in step 2 under stirring condition , stirred and reacted for 2 hours at a temperature of 25°C, filtered the reaction solution after the reaction, and obtained 5.20 g of orange-red [1,1'-bis(diphenylphosphino)ferrocene]dichloropalladium dichloromethane complex The compound crystallized with a yield of 93.89%.

[0031] In this embodiment, dichloromethane is directly used as a solvent, and the target product [1,1'-bis(diphenylphosphino)ferrocene]dichloropalladium dichloro...

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Abstract

The invention discloses a synthetic method of a [1,1'- bis-(diphenyl phosphine) ferrocene] palladium dichloride methylene dichloride complex. The synthetic method comprises the following steps of: dissolving sodium chloropalladite to absolute ethyl alcohol to obtain an ethanol solution of the sodium chloropalladite; dissolving 1,1'- bis-(diphenyl phosphine) ferrocene to methylene dichloride to obtain a methylene dichloride solution of the 1,1'- bis-(diphenyl phosphine) ferrocene; and dropwise adding the ethanol solution of the sodium chloropalladite to the methylene dichloride solution of the 1,1'- bis-(diphenyl phosphine) ferrocene for stirring, reacting and filtering to obtain orange red [1,1'- bis-(diphenyl phosphine) ferrocene] palladium dichloride methylene dichloride complex crystal. In the synthetic method, the methylene dichloride is directly used as a solvent, a target product of the solvent complex is obtained through one-step synthesis, the reaction process is simple, the synthetic cycle is short, the production cost is low, the operation is easy, the reaction condition is mild, the product is precipitated in a crystal form, the purity is larger than 99%, and the yield is larger than 90%.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a synthesis method of [1,1'-bis(diphenylphosphino)ferrocene]dichloropalladium dichloromethane complex. Background technique [0002] Various phosphine bridge transition dinuclear complexes mainly based on bidentate phosphine ligands have attracted great interest from researchers due to their special structure and novel catalytic performance. Ferrocene has also been attracted by its special molecular structure. widespread attention of the people. 1,1′-bis(diphenylphosphino)ferrocene (dppf) is a novel ligand that combines an organic bidentate phosphine ligand with ferrocene, and has a specific flexible framework that can interact with another transition metal atom Form a variety of bimetallic and multimetallic complexes. These complexes are widely used in catalytic hydrogenation, C-C coupling, hydrosilylation of ketones and other reactions. [0003] [1,1'-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F19/00
Inventor 王昭文潘丽娟卢新宁谭小艳张之翔
Owner XIAN CATALYST NEW MATERIALS CO LTD
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