Amphiphilic tb(Ⅲ) complexes, preparation methods thereof, and preparation methods and applications of fluorescent nanofibers

A technology of fluorescent nanofibers and complexes, applied in the direction of steroids, fluorescence/phosphorescence, chemical instruments and methods, etc., to achieve the effects of mild reaction conditions, simple preparation methods, and easy operation

Inactive Publication Date: 2016-05-11
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although lanthanide metal complexes have been widely used in the detection of anions, the comprehensive performance of such sensors, such as: selectivity, sensitivity, still needs to be further improved, and ATA sensors based on such compounds are rarely reported

Method used

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  • Amphiphilic tb(Ⅲ) complexes, preparation methods thereof, and preparation methods and applications of fluorescent nanofibers
  • Amphiphilic tb(Ⅲ) complexes, preparation methods thereof, and preparation methods and applications of fluorescent nanofibers
  • Amphiphilic tb(Ⅲ) complexes, preparation methods thereof, and preparation methods and applications of fluorescent nanofibers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] (1) Synthesis of 6-hydroxymethyl-2-formic acid ethyl pyridine

[0051] Under a nitrogen gas flow rate of 1 mL / s, 5 g of ethyl 2,6-dicarboxylate pyridine and 0.424 g of sodium borohydride were added to a round-bottomed flask filled with 95 mL of absolute ethanol, and ethyl 2,6-dicarboxylate The molar ratio of pyridine and sodium borohydride is 1:0.5. Reflux at 90°C for 5 hours, then adjust the pH value to 5, extract with chloroform, dry over anhydrous sodium sulfate, remove chloroform by rotary evaporation, and use a mixture of methanol and chloroform at a volume ratio of 1:15 Use the mobile phase and silica gel as the stationary phase for column chromatography to obtain 6-hydroxymethyl-2-formic acid ethyl pyridine.

[0052] 1 H-NMR, δ H (400MHz, CDCl 3 , Me 4 Si): 1.43 (3H, O-CH 2 - CH 3 ), 4.47 (2H, O- CH 2 -CH 3 ), 4.87(2H, CH 2 -OH), 7.52 (1H, pyridineprotons), 7.85 (1H, pyridineprotons), 8.03 (1H, pyridineprotons). Its reaction equation is as follow...

Embodiment 2

[0078] (1) Synthesis of 6-hydroxymethyl-2-formic acid ethyl pyridine

[0079] Under a nitrogen gas flow rate of 1 mL / s, 5 g of ethyl 2,6-dicarboxylate pyridine and 0.505 g of sodium borohydride were added to a round-bottomed flask filled with 125 mL of absolute ethanol, and ethyl 2,6-dicarboxylate The molar ratio of pyridine and sodium borohydride is 1:0.6, reflux reaction at 90°C for 5 hours, then adjust the pH to about 5, extract with chloroform, dry over anhydrous sodium sulfate, remove chloroform by rotary evaporation, and use methanol and tris The mixed liquid with a volume ratio of 1:15 of methyl chloride was used as the mobile phase, and silica gel was used as the stationary phase for column chromatography to obtain 6-hydroxymethyl-2-formic acid ethyl pyridine. 1 H-NMR, δ H (400MHz, CDCl 3 , Me 4 Si): 1.43 (3H, O-CH 2 - CH 3 ), 4.47 (2H, O- CH 2 -CH 3 ), 4.87(2H, CH 2 -OH), 7.52 (1H, pyridineprotons), 7.85 (1H, pyridineprotons), 8.03 (1H, pyridineprotons)....

Embodiment 3

[0096] (1) Synthesis of 6-hydroxymethyl-2-formic acid ethyl pyridine

[0097] Under the condition of nitrogen gas with a flow rate of 1.2mL / s, 5g of ethylpyridine 2,6-dicarboxylate and 0.509g of sodium borohydride were added to a round-bottomed flask filled with 130mL of absolute ethanol, and ethyl 2,6-dicarboxylate The molar ratio of ester pyridine to sodium borohydride is 1:0.7. Reflux reaction at 90°C for 5h, then adjust the pH to 5, extract with chloroform, dry over anhydrous sodium sulfate, remove chloroform by rotary evaporation, and use methanol and tris The mixed liquid with a volume ratio of 1:15 of methyl chloride was used as the mobile phase, and silica gel was used as the stationary phase for column chromatography to obtain 6-hydroxymethyl-2-formic acid ethyl pyridine. 1 H-NMR, δ H (400MHz, CDCl 3 , Me 4 Si): 1.43 (3H, O-CH 2 - CH 3 ), 4.47 (2H, O- CH 2 -CH 3 ), 4.87(2H, CH 2 -OH), 7.52 (1H, pyridineprotons), 7.85 (1H, pyridineprotons), 8.03 (1H, pyri...

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Abstract

The invention relates to an amphiphilic Tb (III) complex, a preparation method thereof and a preparation method and application of fluorescent nano-fibers. By virtue of characteristics of a rigid framework, biocompatibility and self-assembling of cholesterol molecules, the amphiphilic Tb (III) complex containing a cholesterol structural unit and bi-picolinic acid is designed and prepared, the supermolecule fluorescent nano-fibers based on the amphiphilic Tb (III) complex are assembled, and action mechanisms of the fluorescent nano-fibers and aurintricarboxylic acid are researched; by virtue of synergetic complexing between aurintricarboxylic acid and ions of Tb (III) and an energy transfer process, aurintricarboxylic acid is efficiently sensed. Related reaction conditions are mild and easy to achieve, the preparation method of the fluorescent nano-fibers is simple, convenient and easy to operate, the prepared fluorescent nano-fibers are uniform in size, the sensitivity for detecting aurintricarboxylic acid is high, the selectivity is good, and the fluorescent nano-fibers are hopeful for being used for researching the pharmaceutical process of aurintricarboxylic acid.

Description

technical field [0001] The invention belongs to the technical field of supramolecular sensing materials, and specifically relates to an amphiphilic Tb(III) complex, a preparation method thereof, and a preparation method and application of fluorescent nanofibers. Background technique [0002] Aurintricarboxylic acid (Aurintricarboxylic acid, ATA) is an aromatic acid derivative, which can inhibit the interaction between protein and nucleic acid in cells, thereby inhibiting cell growth and division. For example: it was found to inhibit the replication of influenza A virus, and it has also been shown to block the invasion of the gp120 molecule on the surface of HIV to the CD4 receptor of T cells. Therefore, ATA is expected to be used in the control and treatment of certain diseases, and monitoring the performance of ATA in living organisms is crucial to the study of the pharmacological process of ATA, so the development of ATA sensors with excellent performance will greatly prom...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J51/00C09K11/06G01N21/64
CPCC07J51/00C09K11/06C09K2211/182G01N21/643
Inventor 刘静王小静雷海瑞严军林刘华卫
Owner SHAANXI NORMAL UNIV
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