Azothiourea anion receptor and preparation method and application thereof

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, strong practicability, the effect of less dosage

Active Publication Date: 2016-04-27
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 receptor and preparation method and application thereof
  • Azothiourea anion receptor and preparation method and application thereof
  • Azothiourea anion receptor and preparation method and application thereof

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 anion receptor, which is characterized in that molecular structural formula of the azothiourea anion receptor is as shown in the formula I. The invention also discloses a preparation method of the above azothiourea anion receptor. By observing ultraviolet spectrum of the anion receptor, whether halogen anion is F<-> can be identified accurately and rapidly, so as to identify whether dicarboxylate anion added is azelaic acid ion. The preparation method of the anion receptor is easy. The detection only needs macroscopic observation and ultraviolet absorption detection. The detection mode is simple and convenient. Dosage of the anion receptor is low, cost is low, and the invention is easy to realize. The product has very strong practicality.

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 Applications(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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