Preparing process of Ru(II) polypyridine complex

A polypyridine and complex technology, which is applied in the field of preparation of ruthenium polypyridine complexes, can solve the problems of weak fluorescence enhancement, limitation and the like

Inactive Publication Date: 2007-06-27
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the potential carcinogenic toxicity of ethidium bromide, the fluorescence enhancement effect of triple-stranded DNA is weaker than that of double-stranded DNA, so ethidium bromide is limited in the detection of triple-stranded DNA

Method used

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  • Preparing process of Ru(II) polypyridine complex
  • Preparing process of Ru(II) polypyridine complex
  • Preparing process of Ru(II) polypyridine complex

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: Ruthenium (II) polypyridine complex preparation:

[0025] 1. Add 15g o-phenanthroline and 8.0g sodium bromide successively in a 250mL flask, add 90mL concentrated sulfuric acid and 45mL concentrated nitric acid while stirring, heat (the temperature is controlled at 120°C or 150°C) and reflux for 50min, and cool to 20 or After 25°C, neutralize with 0% sodium hydroxide, extract the filtered filtrate with dichloromethane, heat the extract to 100°C, evaporate to dryness and recrystallize with methanol to obtain 1,10-phenanthroline-5 , 6-diquinone product;

[0026] 2. Add 0.5g of 1,10-phenanthroline-5,6-diquinone and o-phenylenediamine to a 250mL flask respectively, then add 100mL of ethanol, heat (the temperature is controlled at 100°C or 110°C) to reflux for 20min, and cool After reaching 15 or 20°C, add 10ml of water to produce a yellow milky precipitate, filter and recrystallize with a mixture of ethanol and water (3:1, v / v) to obtain yellow needle-like cr...

Embodiment 2

[0029] Embodiment 2: Ruthenium (II) polypyridine complex preparation:

[0030] 1. Add 15g o-phenanthroline and 8.0g sodium bromide successively in a 250mL flask, add 90mL concentrated sulfuric acid and 45mL concentrated nitric acid while stirring, heat (the temperature is controlled at 120°C or 150°C) and reflux for 50min, and cool to 20 or After 25°C, neutralize with 30% sodium hydroxide, extract the filtered filtrate with dichloromethane, heat the extract to 100°C, evaporate to dryness and recrystallize with methanol to obtain 1,10-phenanthroline-5 , 6-diquinone product;

[0031] 2. Add 0.5g 1,10-phenanthroline-5,6-diquinone and 4,5-dimethyl-o-phenylenediamine respectively in a 250mL flask, then add 100mL ethanol and heat (the temperature is controlled at 110°C or 130°C) for reflux for 20min, cooled to 15 or 20°C, adding 10ml of water to produce a yellow milky precipitate, filtered and recrystallized with a mixture of ethanol and water (3:1, v / v) to obtain a yellow needle ...

Embodiment 3

[0034] Embodiment 3: Ruthenium (II) polypyridine complex preparation:

[0035] 1. Add 15g o-phenanthroline and 8.0g sodium bromide successively into a 250mL flask, add 90mL concentrated sulfuric acid and 45mL concentrated nitric acid while stirring, heat (the temperature is controlled at 120°C or 150°C) and reflux for 50min, and cool to 20°C Or after 25°C, neutralize with 30% sodium hydroxide, extract the filtered filtrate with dichloromethane, heat the extract to 100°C, evaporate to dryness and recrystallize with methanol to obtain 1,10-phenanthroline- 5,6-Diquinone product;

[0036] 2. Add 0.5g of 1,10-phenanthroline-5,6-diquinone and o-phenylenediamine to a 250mL flask respectively, then add 100mL of ethanol, heat (the temperature is controlled at 100°C or 110°C) to reflux for 20min, and cool After reaching 15°C or 20°C, add 10ml of water to produce a yellow milky precipitate, filter and recrystallize with a mixture of ethanol and water (3:1, v / v) to obtain yellow needle-l...

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Abstract

The preparation process of Ru(II)-polypyridine complex includes the following steps: preparing 1,10-phenanthroline-5,6-diquinone, pyridine [3, 2-a:2', 3'-c] phenazine as ligand I, and 7,8-dimethyl pyridine [3, 2-a: 2', 3'-c] phenazine as ligand II, Ru(bipy)2Cl2.2H2O (bipy=2, 2'-dipyridyl) as precursor I and Ru(phen)2Cl2.2H2O as precursor II; adding certain amount of Ru(bipy)2Cl2.2H2O/Ru(phen)2Cl2.2H2O, ligand I/ligand II, and mixture liquid of methanol and water, heating reflux for certain time, heating to concentrate, adding water and boiling, freezing, adding sodium tetrafluoborate, filtering and separating out precipitate, re-crystallization in alcohol, and stoving under infrared lamp to obtain the Ru(II)-polypyridine complex. The Ru(II)-polypyridine complex is used as nucleic acid recognizing probe for the analysis and detection of nucleic acid, and has high stability, high sensitivity, high selectivity and other advantages.

Description

technical field [0001] The invention belongs to the field of synthesis of transition metal complexes, and more specifically relates to a preparation method of a ruthenium (II) polypyridine complex, which is suitable for nucleic acid quantification, base mismatch and triple helix DNA detection. Background technique [0002] Ru(bipy) Polypyridine Complexes of Ruthenium(II) 2 (dppz) 2+ and Ru(phen) 2 (dppz) 2+ There is no fluorescence in aqueous solution, and the fluorescence can be enhanced by 10 after combining with double-stranded DNA 4 times, so it is vividly called the "optical switch" of nucleic acid molecules. They are a new type of highly sensitive fluorescent probes, which have a strong ability to recognize different configurations and different base contents of nucleic acids, and can not only distinguish DNA and RNA, but also B-DNA, Z-DNA and A-DNA , poly(AT) and poly(GC), can also distinguish single-stranded DNA and double-stranded DNA, and can also be used for ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00G01N33/52C12Q1/68
Inventor 何治柯凌连生黄珊吉邢虎
Owner WUHAN UNIV
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