CN101503428A - Method for preparing platinum complex - Google Patents
Method for preparing platinum complex Download PDFInfo
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- CN101503428A CN101503428A CNA2008102365211A CN200810236521A CN101503428A CN 101503428 A CN101503428 A CN 101503428A CN A2008102365211 A CNA2008102365211 A CN A2008102365211A CN 200810236521 A CN200810236521 A CN 200810236521A CN 101503428 A CN101503428 A CN 101503428A
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Abstract
The invention provides a preparation method of palladium coordination compound, which comprises the following steps: dissolving inorganic palladium salt PdCl2 in an organic solvent to obtain an A solution; dissolving dppf in a solvent to obtain a B solution; adding the A solution into the B solution or adding the B solution into the A solution, stirring continuously, and filtering after reacting for 1.5-5 hours to obtain a salmon pink crystal Pd(dppf)Cl2; wherein Pd is bivalence palladium ion, dppf is 1,1-bi(diphenylphosphine)dicyclopentadienyl iron, the organic solvent is one or mixing solution of two of anhydrousl alcohol, tetrahydrofuran and toluol. The invention has the advantages of simple operation, easily-obtained raw materials and low cost, and the obtained product is separated out in form of crystal and has high purity and yield rate. In addition, the palladium coordination compound prepared in the invention can stably exist in the natural condition and plays a role of catalyzation in carbonylation reaction, cross-coupling reaction and suzuki coupling reaction.
Description
Technical field
The present invention relates to a kind of preparation method of metal complexes, be specifically related to a kind of preparation method of palladium complex.
Background technology
In all transition metal, the application of palladium in organic synthesis is the most extensive, the organic palladium title complex can be accepted many different types of functional groups, can promote the reaction of various generation C-C keys and other key, and these reactions often has higher chemo-selective and regioselectivity.Based on the various phosphine bridge transition dinuclear complexs of bidentate phosphine ligands because its special construction, novel reactivity worth and catalysis behavior, be subjected to people's common concern, become the field, a forward position of Organometallic Chemistry, 1, two (diphenylphosphine) ferrocene of 1-can be used as a bidentate phosphine ligands with potential use, can form various bimetals and multi-metal complex with another transition metal atoms again.1, two (diphenylphosphine) ferrocene of 1-promptly might generate double-core or polynuclear coordination compound, and this class title complex demonstrate their important use at aspects such as catalysis, organic synthesis, biological enzymes day by day when doing the time spent with another monokaryon transition metal complex.
Palladium ion and 1, the reaction of two (diphenylphosphine) ferrocene of 1-also had relevant bibliographical information in the past, but preparation method's complexity is raw materials used rare, the process complexity.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of simple to operate at above-mentioned deficiency of the prior art, and cost is low, the preparation method of the palladium complex that the product purity of productive rate height and preparation is big.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of palladium complex is characterized in that preparation process is: with inorganic palladium salt PdCl
2Be dissolved in and obtain A solution in the organic solvent, dppf is dissolved in obtains B solution in the solvent, described A solution is added in the described B solution or with described B solution add in the described A solution, constantly stir, react 1.5-5 hour after-filtration, obtain orange red crystallization Pd (dppf) Cl
2, wherein, Pd is the divalence palladium ion, dppf is 1, two (diphenylphosphine) ferrocene of 1-; Described organic solvent is one or more mixed solvents in dehydrated alcohol, tetrahydrofuran (THF) or the toluene.
Described PdCl
2With the mol ratio of dppf be 1: 1-1.2.
The volume ratio of described A solution and B solution is 1: 1.5-3.
The present invention compared with prior art has the following advantages: the present invention is simple to operate, and synthesis material is easy to get, and cost is low, and the product of preparation is separated out with crystalline form, and purity is big, the productive rate height; And the palladium complex of the present invention's preparation energy stable existence under state of nature, in carbonylation reaction, cross-coupling reaction, suzuki reaction, present good katalysis.
Below by embodiment, technical scheme of the present invention is described in further detail.
Description of drawings
Fig. 1 is the infrared spectrogram of the resulting title complex of the embodiment of the invention.
Embodiment
The structural formula of the palladium complex of the present invention's preparation is: Pd (dppf) Cl
2, wherein, Pd is the divalence palladium ion, dppf is 1, two (diphenylphosphine) ferrocene of 1-.
Concrete preparation method is: with inorganic palladium salt PdCl
2Be dissolved in and obtain A solution in the organic solvent, dppf is dissolved in obtains B solution in the solvent, described A solution is added in the described B solution or with described B solution add in the described A solution, constantly stir, react 1.5-5 hour after-filtration, obtain orange red crystallization Pd (dppf) Cl
2, wherein, Pd is the divalence palladium ion, dppf is 1, two (diphenylphosphine) ferrocene of 1-; Described organic solvent is one or more mixed solvents in dehydrated alcohol, tetrahydrofuran (THF) or the toluene.Described PdCl
2With the mol ratio of dppf be 1: 1-1.2; The volume ratio of described A solution and B solution is 1: 1.5-3.
Embodiment 1
With 0.2gPdCl
2Be dissolved in and get A solution in the 30mL dehydrated alcohol, 0.8gdppf is dissolved in gets B solution in the 50mL tetrahydrofuran (THF), A solution is added in the B solution, constantly stir, react the 3h after-filtration, obtain orange red crystallization, yield 98%, purity is 99%.
Ultimate analysis: calculated value, C55.78, H3.83; Experimental value, C55.71, H3.85, its infrared spectra is seen Fig. 1.
Embodiment 2: the preparation of title complex
With 0.2gPdCl
2Be dissolved in (A solution) in the 30mL dehydrated alcohol, 0.8g dppf is dissolved in (B solution) in the 50mL tetrahydrofuran (THF), and B adds among the A, constantly stirs, and reaction 3h after-filtration obtains orange red crystallization, yield 98%, and purity is 99%.
Ultimate analysis: calculated value, C55.78, H3.83; Experimental value, C55.71, H3.85, its infrared spectra is seen Fig. 1.
Embodiment 3: the preparation of title complex
With 0.2gPdCl
2Be dissolved in (A solution) in the 30mL dehydrated alcohol, 0.6g dppf is dissolved in (B solution) in the 45mL tetrahydrofuran (THF), and A adds among the B, constantly stirs, and reaction 3h after-filtration obtains orange red crystallization, yield 95%, and purity is 99%.
Ultimate analysis: calculated value, C55.78, H3.83; Experimental value, C55.71, H3.85, its infrared spectra is seen Fig. 1.
Embodiment 4: the preparation of title complex
With 0.2gPdCl
2Be dissolved in (A solution) in the 30mL dehydrated alcohol, 0.6g dppf is dissolved in (B solution) in the 45mL tetrahydrofuran (THF), and A adds among the B, constantly stirs, and reaction 1.5h after-filtration obtains orange red crystallization, yield 94%, and purity is 99%.
Ultimate analysis: calculated value, C55.78, H3.83; Experimental value, C55.71, H3.85, its infrared spectra is seen Fig. 1.
Embodiment 5: the preparation of title complex
With 0.2gPdCl
2Be dissolved in (A solution) in the 30mL dehydrated alcohol, 0.8g dppf is dissolved in (B solution) in the 50mL tetrahydrofuran (THF), and A adds among the B, constantly stirs, and reaction 5h after-filtration obtains orange red crystallization, yield 98%, and purity is 99%.
Ultimate analysis: calculated value, C55.78, H3.83; Experimental value, C55.71, H3.85, its infrared spectra is seen Fig. 1.
Claims (3)
1. the preparation method of a palladium complex is characterized in that preparation process is: with inorganic palladium salt PdCl
2Be dissolved in and obtain A solution in the organic solvent, dppf is dissolved in obtains B solution in the solvent, described A solution is added in the described B solution or with described B solution add in the described A solution, constantly stir, react 1.5-5 hour after-filtration, obtain orange red crystallization Pd (dppf) Cl
2, wherein, Pd is the divalence palladium ion, dppf is 1, two (diphenylphosphine) ferrocene of 1-; Described organic solvent is one or more mixed solvents in dehydrated alcohol, tetrahydrofuran (THF) or the toluene.
2. the preparation method of a kind of palladium complex according to claim 1 is characterized in that: described PdCl
2With the mol ratio of dppf be 1: 1-1.2.
3. the preparation method of a kind of palladium complex according to claim 1, it is characterized in that: the volume ratio of described A solution and B solution is 1: 1.5-3.
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| CN2008102365211A CN101503428B (en) | 2008-12-30 | 2008-12-30 | Method for preparing platinum complex |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101863926A (en) * | 2010-06-18 | 2010-10-20 | 河北大学 | Antitumor drug palladium coordination compound |
| CN102603811A (en) * | 2012-02-22 | 2012-07-25 | 西安凯立化工有限公司 | Synthetic method of [1,1'- bis-(diphenyl phosphine) ferrocene] palladium dichloride methylene dichloride complex |
| CN102786552A (en) * | 2012-08-08 | 2012-11-21 | 陕西瑞科新材料股份有限公司 | Preparation method of [1,1'-di(diphenyl phosphino) ferrocene] palladium dichloride (dppfPdCl2) |
| CN108291306A (en) * | 2015-11-27 | 2018-07-17 | 埃托特克德国有限公司 | Electroless plated bath compositions and method for palladium |
| CN111253446A (en) * | 2019-12-11 | 2020-06-09 | 江苏欣诺科催化剂有限公司 | Preparation method of palladium complex |
-
2008
- 2008-12-30 CN CN2008102365211A patent/CN101503428B/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101863926A (en) * | 2010-06-18 | 2010-10-20 | 河北大学 | Antitumor drug palladium coordination compound |
| CN101863926B (en) * | 2010-06-18 | 2013-04-10 | 河北大学 | Antitumor drug palladium coordination compound |
| CN102603811A (en) * | 2012-02-22 | 2012-07-25 | 西安凯立化工有限公司 | Synthetic method of [1,1'- bis-(diphenyl phosphine) ferrocene] palladium dichloride methylene dichloride complex |
| CN102603811B (en) * | 2012-02-22 | 2014-09-03 | 西安凯立化工有限公司 | Synthetic method of [1,1'- bis-(diphenyl phosphine) ferrocene] palladium dichloride methylene dichloride complex |
| CN102786552A (en) * | 2012-08-08 | 2012-11-21 | 陕西瑞科新材料股份有限公司 | Preparation method of [1,1'-di(diphenyl phosphino) ferrocene] palladium dichloride (dppfPdCl2) |
| CN108291306A (en) * | 2015-11-27 | 2018-07-17 | 埃托特克德国有限公司 | Electroless plated bath compositions and method for palladium |
| CN108291306B (en) * | 2015-11-27 | 2019-12-27 | 埃托特克德国有限公司 | Plating bath composition and method for electroless plating of palladium |
| CN111253446A (en) * | 2019-12-11 | 2020-06-09 | 江苏欣诺科催化剂有限公司 | Preparation method of palladium complex |
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| CN101503428B (en) | 2011-12-07 |
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