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

A technology of dichloromethane and diphenylphosphine, applied in the field of [1], can solve the problems of cumbersome preparation process and high production cost, and achieve the effect of simple reaction process, low production cost and mild reaction conditions

Active Publication Date: 2014-09-03
XIAN CATALYST NEW MATERIALS CO LTD
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  • Abstract
  • Description
  • Claims
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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

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Step 1. Dissolve 2.00 grams of sodium chloropalladite in 30 mL of absolute ethanol to obtain an ethanol solution of sodium chloropalladite;

[0018] Step 2. Dissolve 4.15 g of 1,1'-bis(diphenylphosphine)ferrocene in 41mL of dichloromethane to obtain a dichloromethane solution of 1,1'-bis(diphenylphosphine)ferrocene ;

[0019] Step 3. Add the ethanol solution of sodium chloropalladite described in step one dropwise to the dichloromethane solution of 1,1'-bis(diphenylphosphine)ferrocene described in step two under stirring conditions , The reaction was stirred for 1 hour at a temperature of 25°C, and the reaction solution was filtered after the reaction to obtain 5.01 g of orange-red [1,1′-bis(diphenylphosphine)ferrocene]dichloropalladium dichloromethane complex The compound crystallized with a yield of 90.46%.

[0020] In this example, dichloromethane was directly used as the solvent to synthesize the target product of the solvent complex [1,1'-bis(diphenylphosphine)ferrocene...

Embodiment 2

[0023] Step 1. Dissolve 2.00 grams of sodium chloropalladite in 40 mL of absolute ethanol to obtain an ethanol solution of sodium chloropalladite;

[0024] Step 2. Dissolve 4.52 g of 1,1'-bis(diphenylphosphine)ferrocene in 45mL of dichloromethane to obtain a dichloromethane solution of 1,1'-bis(diphenylphosphine)ferrocene ;

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

[0026] In this example, dichloromethane was directly used as the solvent to synthesize the target product of the solvent complex [1,1'-bis(diphenylphosphine)ferrocene] d...

Embodiment 3

[0028] Step 1. Dissolve 2.00 grams of sodium chloropalladite in 20 mL of absolute ethanol to obtain an ethanol solution of sodium chloropalladite;

[0029] Step 2. Dissolve 4.15 g of 1,1'-bis(diphenylphosphine)ferrocene in 21mL of dichloromethane to obtain a dichloromethane solution of 1,1'-bis(diphenylphosphine)ferrocene ;

[0030] Step 3. Add the ethanol solution of sodium chloropalladite described in step 1 dropwise to the dichloromethane solution of 1,1'-bis(diphenylphosphine)ferrocene described in step 2, under stirring conditions , The reaction was stirred for 2h at a temperature of 25℃. After the reaction, the reaction solution was filtered to obtain 5.20 g of orange-red [1,1′-bis(diphenylphosphine)ferrocene]dichloropalladium dichloromethane complex The compound crystallized with a yield of 93.89%.

[0031] In this example, dichloromethane was directly used as the solvent to synthesize the target product of the solvent complex [1,1'-bis(diphenylphosphine)ferrocene] dichlorop...

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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 specifically relates to a method for synthesizing a [1,1'-bis(diphenylphosphine)ferrocene] dichloropalladium dichloromethane complex. Background technique [0002] Various phosphine bridge transition dinuclear complexes based on bidentate phosphine ligands have a special structure and novel catalytic reaction performance, which arouses great interest of researchers. Ferrocene has also been attracted by its special molecular structure. People's widespread attention. 1,1'-Bis(diphenylphosphine)ferrocene (dppf) is a new type of ligand that combines organic bidentate phosphine ligands with ferrocene. It has a specific flexible framework and can interact with another transition metal atom. Form a variety of bimetal and multimetal complexes. Such complexes are widely used in catalytic hydrogenation, C-C coupling, and hydrosilylation of ketones. [0003] [1,1'-Bis(diphenylphosphine)ferrocene]...

Claims

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Application Information

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Patent Type & Authority Patents(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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