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A kind of dinuclear ruthenium nnn complex and preparation method thereof

A technology for binuclear ruthenium and complexes, which is applied in the field of binuclear ruthenium NNN complexes and their preparation, can solve problems such as easy deactivation and unfavorable polymerization reaction, and achieve the effects of easy storage, simple synthesis route and air insensitivity.

Inactive Publication Date: 2018-05-15
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this kind of binuclear nickel metal complex is easily deactivated at a temperature higher than 50 °C, which is not conducive to catalyzing the polymerization reaction at high temperature

Method used

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  • A kind of dinuclear ruthenium nnn complex and preparation method thereof
  • A kind of dinuclear ruthenium nnn complex and preparation method thereof
  • A kind of dinuclear ruthenium nnn complex and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023]

[0024] Under nitrogen conditions, coordinate unsaturated mononuclear ruthenium metal complex 2 (69mg, 0.1mmol), 1,3-bis(4-pyridine)propane 3a (10mg, 0.05mmol), in 2mL ethanol solvent 78℃ Stir for 1h. Remove volatile components under reduced pressure, use CH for solid 2 Cl 2 / N-hexane (v:v=1:2) was recrystallized to obtain a reddish-brown solid as the target product 1a (72 mg, yield 92%). The target product was confirmed by nuclear magnetic resonance spectroscopy and elemental analysis.

Embodiment 2

[0026] The reaction steps and operations are the same as in Example 1, and the difference from Example 1 is that the reaction time of the system is 24h. After the reaction was stopped, a reddish brown solid was obtained as the target product 1a (70 mg, yield 89%) after post-treatment. It shows that extending the reaction time is not beneficial to increasing the yield of the target product.

Embodiment 3

[0028] The reaction steps and operations are the same as in Example 1, and the difference from Example 1 is that the reaction solvent is toluene and the reaction temperature is 110°C. After the reaction was stopped, a reddish brown solid was obtained as the target product 1a (55 mg, yield 69%) after post-treatment. It shows that this reaction can also be carried out in aprotic solvents.

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Abstract

The invention discloses a binuclear ruthenium NNN complex and a preparation method thereof. Coordinated unsaturated mononuclear ruthenium metal complexes and nitrogen-containing bidentate ligands undergo a coordination reaction in an organic solvent at a molar ratio of 2:1. After the reaction, a simple post-treatment is performed to obtain dinuclear ruthenium with high catalytic activity. NNN complexes. The invention has the advantages of simple operation, mild reaction conditions, high synthesis efficiency and the like.

Description

Technical field [0001] The invention relates to a binuclear ruthenium NNN complex and a preparation method thereof. The coordination unsaturated mononuclear ruthenium metal complex is used as a raw material, and it is coordinated with a nitrogen-containing bidentate ligand in an organic solvent at a 2:1 molar ratio Reaction to synthesize a binuclear ruthenium NNN complex with higher catalytic activity. The invention has the advantages of simple operation, mild reaction conditions, high synthesis efficiency and the like. technical background [0002] Pyridyl nitrogen heterocyclic ligands are easily coordinated with transition metals, and the metal complexes formed are relatively stable. They have been successfully used in cross-coupling, catalytic hydrogenation, Michael addition, cyclopropanation, allyl substitution and other reactions. [0003] In recent years, binuclear metal complexes have received extensive attention. Researchers have found that binuclear metal complexes have h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F15/00B01J31/22C07C33/20C07C29/143
Inventor 余正坤刘婷婷
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI