Intermediate for synthesizing benzothiadiazole malononitrile, synthesis method thereof and method for detecting CN<->

A technology of benzothiadiazole malononitrile and synthesis method, which is applied in the field of CN-detection and can solve problems such as rapid poisoning

Active Publication Date: 2018-12-14
FUYANG NORMAL UNIVERSITY
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Problems solved by technology

But cyanide is a highly toxic substance, and it gets poisoned very quickly

Method used

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  • Intermediate for synthesizing benzothiadiazole malononitrile, synthesis method thereof and method for detecting CN&lt;-&gt;
  • Intermediate for synthesizing benzothiadiazole malononitrile, synthesis method thereof and method for detecting CN&lt;-&gt;
  • Intermediate for synthesizing benzothiadiazole malononitrile, synthesis method thereof and method for detecting CN&lt;-&gt;

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Embodiment Construction

[0047] 1. be used for the intermediate of synthetic benzothiadiazole malononitrile, as shown in formula (Ⅲ):

[0048]

[0049] 2. For the synthesis of the intermediate of benzothiadiazole malononitrile and the synthetic method of benzothiadiazole malononitrile, the synthetic route is as follows figure 1 shown, including the following steps:

[0050] (1) Synthesis of intermediate TPA-BTD-Br;

[0051] Place 2.7568g of 4-dianilinophenylboronic acid, 2.3576g of 4,7-dibromo-2,1,3-benzothiadiazole, 0.1342g of 4-(triphenylphosphine) palladium and 1.7880g of potassium carbonate In a 250mL three-neck flask, add 60mL tetrahydrofuran THF, 45mL toluene and 22mL distilled H2O to the mixture. 2 O, then add 0.1mL methyl trioctyl ammonium chloride dropwise; add a magnet and stir fully, reflux reaction under nitrogen atmosphere for 16h, the temperature of reflux reaction is 85°C; after the reaction, add 200mL distilled water to the reactant, and then Extract the organic phase with dichlo...

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Abstract

The invention discloses an intermediate for synthesizing benzothiadiazole malononitrile, a synthesis method thereof and a method for detecting CN<->. The intermediate for synthesizing the benzothiadiazole malononitrile is shown as a formula (III): FORMULA. The synthesis method of the intermediate shown as the formula (III) comprises the following steps: (1), synthesizing an intermediate TPA-BTD-Br; (2), synthesizing the intermediate TPA-BTD-CHO shown as the formula (III). The method for detecting the CN<-> comprises the following steps: (1), with tetrahydrofuran THF as a solvent, adding benzothiadiazole malononitrile TPA-BTD-BT to obtain a tetrahydrofuran THF solution of the benzothiadiazole malononitrile TPA-BTD-BT; (2), adding a sample to be detected into the tetrahydrofuran THF solutionof the benzothiadiazole malononitrile TPA-BTD-BT; (3) identifying whether the CN<-> exists in the sample to be detected through visual observation, UV-vis absorption spectra or fluorescence spectra.The intermediate shown as the formula (III) can be applied to construction of a fluorescent sensor with turn-on-type high selectivity and strong anti-interference ability to the CN<->.

Description

technical field [0001] The invention relates to CN - detection technology field. Specifically, it is an intermediate for synthesizing benzothiadiazole malononitrile and its synthetic method and detection CN - Methods. Background technique [0002] Cyanide is widely used in industrial production and daily life, and can be used in electroplating, plastic manufacturing, metallurgy, gold extraction and tanning in industrial production. But cyanide is a highly toxic substance, and poisoning happens very quickly. They can enter the human body through many ways, such as skin absorption, wound entry, respiratory inhalation, etc. After entering the human body, they can poison the hemoglobin in the blood, resulting in difficulty in breathing and suffocation due to lack of oxygen in cells. Adult oral administration of 150-250mg can cause death. Therefore, the development of a rapid and accurate detection of CN - The method of ions is very interesting. In the past few decades, flu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D285/14C09K11/06G01N21/33G01N21/64G01N24/08
CPCC07D285/14C09K11/06C09K2211/1007C09K2211/1014C09K2211/1051G01N21/33G01N21/64G01N24/088
Inventor 凡素华陈志勇伍敏志
Owner FUYANG NORMAL UNIVERSITY
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