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Azothiourea anion acceptor and its preparation method and application

A technology of azothiourea and anion, which is applied in the direction of analyzing materials through chemical reactions, observing the influence of chemical indicators on materials, organic chemistry, etc., can solve the problems of complex preparation methods, and achieve the goal of preparation methods Easy, less dosage, simple detection method

Active Publication Date: 2017-08-08
JIANGHAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN102241698A reports a technology for fluoride ion detection, but this patent can only detect fluoride ions, and the preparation method is complicated
At present, there is no report on the anion detection of dicarboxylate

Method used

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  • Azothiourea anion acceptor and its preparation method and application
  • Azothiourea anion acceptor and its preparation method and application
  • Azothiourea anion acceptor and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) firstly obtain 3,5-dichloro-4 (2,6-dichloro-4-amino) azoaniline by diazotization reaction of 2,6-dichloro-p-nitroaniline, and then 3,5 -Dichloro-4(2,6-dichloro-4-amino)azoaniline was dissolved in a mixed solvent of methanol (MeOH) and ethyl acetate (EA) with a volume ratio of 3:1, and then 5 molar equivalents of N-butyl isothiocyanate undergoes a substitution reaction, and reacts at 70°C for 12 hours to obtain a mixture of monosubstituted azothiourea products and disubstituted azothiourea products. TLC spot plate tracking found that no matter how long the reaction time was, the disubstituted product was still only about 10%, and the monosubstituted product was about 90%.

[0033] (2) Utilize the chromatographic column to separate the above-mentioned monosubstituted azothiourea product and the double-substituted azothiourea product, the eluent used is the mixed solution of sherwood oil (PE) and ethyl acetate (EA), eluent The volume ratio is from PE:EA=20:1 to PE:EA=...

Embodiment 2

[0036] (1) firstly obtain 3,5-dichloro-4 (2,6-dichloro-4-amino) azoaniline by diazotization reaction of 2,6-dichloro-p-nitroaniline, and then 3,5 -Dichloro-4(2,6-dichloro-4-amino)azoaniline was dissolved in a mixed solvent of methanol (MeOH) and ethyl acetate (EA) with a volume ratio of 1:1, and then 2 molar equivalents of N-butyl isothiocyanate undergoes a substitution reaction, and reacts at 60° C. for 24 hours to obtain a mixture of monosubstituted azothiourea products and disubstituted azothiourea products. TLC spot plate tracking found that no matter how long the reaction time was, the disubstituted product was still only about 10%, and the monosubstituted product was about 90%.

[0037] (2) Utilize the chromatographic column to separate the above-mentioned monosubstituted azothiourea product and the double-substituted azothiourea product, the eluent used is the mixed solution of sherwood oil (PE) and ethyl acetate (EA), eluent The volume ratio is from PE:EA=20:1 to PE:E...

Embodiment 3

[0040] (1) firstly obtain 3,5-dichloro-4 (2,6-dichloro-4-amino) azoaniline by diazotization reaction of 2,6-dichloro-p-nitroaniline, and then 3,5 -Dichloro-4(2,6-dichloro-4-amino)azoaniline was dissolved in a mixed solvent of methanol (MeOH) and ethyl acetate (EA) with a volume ratio of 10:1, and then 10 molar equivalents of N-butyl isothiocyanate undergoes a substitution reaction, reacting at 80° C. for 8 hours to obtain a mixture of monosubstituted azothiourea products and disubstituted azothiourea products. TLC spot plate tracking found that no matter how long the reaction time was, the disubstituted product was still only about 10%, and the monosubstituted product was about 90%.

[0041] (2) Utilize the chromatographic column to separate the above-mentioned monosubstituted azothiourea product and the double-substituted azothiourea product, the eluent used is the mixed solution of sherwood oil (PE) and ethyl acetate (EA), eluent The volume ratio is from PE:EA=20:1 to PE:EA...

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Abstract

The invention discloses an azothiourea-type anion receptor, which is characterized in that: the molecular structure formula of the azothiourea-type anion receptor is shown in formula 1. The invention also discloses a preparation method of the azothiourea anion acceptor. The present invention can accurately and rapidly identify whether the halogen anion is F- by observing the ultraviolet spectrum of the anion acceptor. At the same time, the azothiourea anion acceptor of the present invention can also convert the anion acceptor into a cis structure under the irradiation of visible light, thereby identifying whether the added dicarboxylic acid anion is azelaic acid ion. The preparation method of the anion receptor of the present invention is easy, and the detection method only needs to be detected by naked eye observation and ultraviolet light absorption detection, the detection method is simple, the anion receptor consumption is small, the cost is low and easy to realize, and it has strong practicability.

Description

technical field [0001] The invention relates to the field of anion receptors, in particular to an azothiourea-type anion receptor and its preparation method and application. Background technique [0002] Anions are ubiquitous in organisms and human environments, so anion recognition plays an important role in the fields of life sciences, medical sciences, and environmental sciences. For example, in life sciences, enzyme substrates and coenzymes are mostly anions, DNA, the carrier of genetic information, is a polyanion, and dicarboxylate anions play an important role in many metabolic processes. In medical science, the determination of chloride ion concentration in the body is also extremely important for the detection and treatment of patients with alveolar fiber disease; acetate can treat uremia, and excess acetate in the body can cause vomiting, low blood pressure and even death. In environmental science, excessive use of phosphorus and nitrogen fertilizers may lead to eu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C335/20G01N21/78G01N21/33
CPCC07C335/20G01N21/33G01N21/78
Inventor 王洪波袁迎雪汪聪茜陈锴涛程俊陈仕炎吴玲芳杨慧敏熊小琦
Owner JIANGHAN UNIVERSITY
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