Symmetrical binuclear ruthenium complex and preparation method utilizing microwave

A technology of dinuclear ruthenium complexes and ruthenium complexes, applied in the field of synthetic chemistry, can solve the problems of microwave synthesis of symmetrical dinuclear ruthenium complexes that have not been reported, and achieve high thermal energy utilization rate, improved conversion rate, easy synthesis and modification Effect

Inactive Publication Date: 2014-12-24
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, there is no report on the preparation method of symmetric dinuclear ruthenium complexes synthesized by microwave in China.

Method used

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  • Symmetrical binuclear ruthenium complex and preparation method utilizing microwave
  • Symmetrical binuclear ruthenium complex and preparation method utilizing microwave
  • Symmetrical binuclear ruthenium complex and preparation method utilizing microwave

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] The symmetrical dinuclear ruthenium complex utilizes a microwave preparation method, and its specific steps are as follows:

[0041] (1) Synthesis of ligand 4-(4-bromophenyl)-2,2:6,2-terpyridine, denoted as tpyBr.

[0042]Synthesis of ligand tpyBr: Dissolve 1g, 5.4mmol of 4-bromobenzaldehyde in 120ml of EtOH, and continuously add 1.31g, 10.8mmol of 2-acetylpyridine (the molar ratio of 4-bromobenzaldehyde to 2-acetylpyridine 1:2), 0.3g, 5.4mmol of KOH and 30ml of NH 4 OH, heated to reflux at 90°C for 24h, then stirred at room temperature for 3 hours, a yellow solid precipitated and was filtered with MeOH and H 2 O washing, the obtained white crude product was recrystallized with MeOH to obtain a high-purity white product tpyBr. 1 H-NMR (500MHz, CDCl 3 ): δ(ppm)= 8.73(2H,d), 8.70(2H,s), 8.68(2H,d), 7.88(2H,m), 7.79(2H,d), 7.65(2H,d), 7.36 (2H,m).

[0043] (2) Synthesis of ligand 4-(2,2';6',2''-terpyridine-4'-phenyl)-diethyl phosphate, denoted as tpyPO(OEt) 2 .

[0...

Embodiment 2

[0056] The symmetrical dinuclear ruthenium complex utilizes a microwave preparation method, and its specific steps are as follows:

[0057] (1) Synthesis of ligand 4-(4-bromophenyl)-2,2:6,2-terpyridine, denoted as tpyBr.

[0058] Synthesis of ligand tpyBr: Dissolve 1.3g, 7.02mmol of 4-bromobenzaldehyde in 120mlEtOH, and continuously add 2.13g, 17.56mmol of 2-acetylpyridine (the moles of 4-bromobenzaldehyde and 2-acetylpyridine ratio of 1:2.5), 0.39g, 7.02mmol of KOH and 30ml of NH 4 OH, heated to reflux at 90°C for 24h, then stirred at room temperature for 3 hours, a yellow solid precipitated and was filtered with MeOH and H 2 O washing, the obtained white crude product was recrystallized with MeOH to obtain a high-purity white product tpyBr.1 H-NMR (500MHz, CDCl 3 ): δ(ppm)=8.75(2H,d), 8.71(2H,s), 8.69(2H,d), 7.83(2H,m), 7.75(2H,d), 7.62(2H,d), 7.37 (2H,m).

[0059] (2) Synthesis of ligand 4-(2,2';6',2''-terpyridine-4'-phenyl)-diethyl phosphate, denoted as tpyPO(OEt) 2 ....

Embodiment 3

[0070] The symmetrical dinuclear ruthenium complex utilizes a microwave preparation method, and its specific steps are as follows:

[0071] (1) Synthesis of ligand 4-(4-bromophenyl)-2,2:6,2-terpyridine, denoted as tpyBr.

[0072] Synthesis of ligand tpyBr: Dissolve 1.8g, 9.7mmol of 4-bromobenzaldehyde in 120ml of EtOH, and continuously add 1.313.41g, 28.13mmol of 2-acetylpyridine (4-bromobenzaldehyde and 2-acetylpyridine The molar ratio is 1:2.9), 0.54g, 9.7mmol of KOH and 30ml of NH 4 OH, heated to reflux at 90°C for 24h, then stirred at room temperature for 3 hours, a yellow solid precipitated and was filtered with MeOH and H 2 O washing, the obtained white crude product was recrystallized with MeOH to obtain a high-purity white product tpyBr. 1 H-NMR (500MHz, CDCl 3 ): δ(ppm)= 8.79(2H,d), 8.72(2H,s), 8.65(2H,d), 7.83(2H,m), 7.78(2H,d), 7.61(2H,d), 7.39 (2H,m).

[0073] (2) Synthesis of ligand 4-(2,2';6',2''-terpyridine-4'-phenyl)-diethyl phosphate, denoted as tpyPO(OEt...

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Abstract

The invention relates to a symmetrical binuclear ruthenium complex and a preparation method utilizing microwave, belonging to the technical field of synthetic chemistry. The preparation method comprises the following steps: firstly reacting 2-acetylpyridine with 4-bromobenzaldehye as a starting raw material, wherein traditional NaOH and CH3OH are respectively replaced with KOH and EtOH to further shorten reaction time; performing cross-coupling reaction to the obtained terpyridyl compound and diethyl phosphite, wherein the P-H bond in diethyl phosphite is cut off by taking triethylamine as a salt base; then synthesizing an intermediate complex together with ruthenium trichloride hydrate RuCl3.3H2O, and then synthesizing a target product under microwave conditions. The complex molecules can be adsorbed onto a conductive substrate such as an ITO and the like by taking phosphoryl groups at two ends of the complex molecules as fixed ligands and layer-by-layer self assembling can be realized, and the symmetrical binuclear ruthenium complex is an excellent photosensitive dye. The symmetrical binuclear ruthenium complex is simple in design synthesis process and low in cost, and the microwave-assisted synthesis technology is fast and efficient.

Description

technical field [0001] The invention relates to a symmetrical dinuclear ruthenium complex and a microwave preparation method, belonging to the technical field of synthetic chemistry. Background technique [0002] In today's society, with the increasingly prominent energy issues, finding clean and sustainable energy has become one of the key issues facing mankind. Among the many clean energy sources, solar energy is favored by researchers because of its universality, harmlessness, huge size and long-lasting nature. Solar energy can be said to be inexhaustible, inexhaustible and has no geographical restrictions, can be directly developed and utilized, without mining and transportation, and the development and utilization of solar energy will not pollute the environment. appears to be particularly important. The dye-sensitized solar cell is a new type of solar cell developed by imitating the principle of photosynthesis, and it is one of the main ways to utilize solar energy. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00C09B57/10H01G9/20
Inventor 王华杨丽李孔斋魏永刚祝星
Owner KUNMING UNIV OF SCI & TECH
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