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Preparation method and application of 2, 6-bis(2,4, 6-triamino-5-pyrimidinazo)benzo(1, 2-d; 4, 5-d) bithiazole

A technology for pyrimidine azo and diaminobenzene, which is applied in the field of disazo compounds, can solve the problems of unsatisfactory sensitivity and selectivity of reagents for detecting heavy metal ions, and achieve the effects of stable test system, high sensitivity and fast response speed.

Inactive Publication Date: 2018-02-23
SHANXI DATONG UNIV
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Problems solved by technology

[0004] The present invention provides a 2,6-bis(2,4,6-triamino-5-pyrimidineazo)benzo(1 , 2-d; 4, 5-d) Preparation method and application of bithiazole

Method used

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  • Preparation method and application of 2, 6-bis(2,4, 6-triamino-5-pyrimidinazo)benzo(1, 2-d; 4, 5-d) bithiazole
  • Preparation method and application of 2, 6-bis(2,4, 6-triamino-5-pyrimidinazo)benzo(1, 2-d; 4, 5-d) bithiazole
  • Preparation method and application of 2, 6-bis(2,4, 6-triamino-5-pyrimidinazo)benzo(1, 2-d; 4, 5-d) bithiazole

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Embodiment 1

[0044] Example 1. One kind of 2,6-bis(2,4,6-triamino-5-pyrimidylazo)benzo(1,2-d; 4,5-d)bithiazole (DTAPABDP), its molecular The structural formula is:

[0045] .

[0046] The preparation method of 2,6-bis(2,4,6-triamino-5-pyrimidylazo)benzo(1,2-d; 4,5-d)bithiazole is as follows:

[0047] (1) Preparation of 2,6-diaminobenzo(1,2-d; 4,5-d)bithiazole

[0048] Add 10.81 g (0.1 mol) of 4,4´-p-phenylenediamine, 150 mL of glacial acetic acid and 70 g of potassium thiocyanate to a dry 500 mL three-necked flask equipped with a reflux condenser with a drying tube and a dropping funnel. Stir at room temperature for 20min, then measure 10mL of bromine and dissolve it in 130mL of glacial acetic acid, add it to the reaction mixture, keep the reaction temperature at 45-55°C, continue stirring for 24h, pour the mixture into cold water, and add to the mixture under stirring Add ammonia water, adjust the pH to 8-9, let it stand, after the solution is cooled, suction filter, wash with water ...

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Abstract

The invention belongs to the field of bis-azo compounds. The problem that in the prior art, the detection of the sensitivity and selectivity of heavy metal ion reagents is not ideal enough can be solved. Firstly, 2,6-diamidobenzo(1,2-d; 4,5-d)bithiazole is prepared from 4,4'-p-phenylenediamine, glacial acetic acid, potassium rhodanide and the like; secondly, 2,2'-[benzo(1,2-d; 4,5-d)bithiazole hydrazone]bimalononitrile is prepared from NaNO2 and other raw materials; finally, 2,6-bis(2,4,6-triamino-5-pyrinideazo)benzo(1,2-d; 4,5-d)bithiazole is obtained after guanidine nitrate and an NaOH ethanol solution react with an ethanol solution of the product obtained through the reaction in the second step. A method for detecting the Cu2+ concentration has the advantages of being rapid in response speed, high in selectivity, high in sensitivity and stable in testing system.

Description

technical field [0001] The invention belongs to the field of disazo compounds, in particular to a 2,6-bis(2,4,6-triamino-5-pyrimidineazo)benzo(1,2-d; 4,5-d ) Preparation method and application of bithiazole. Background technique [0002] Heterocyclic azo reagents are an important branch of azo organic reagents, and their structural formula can be simply expressed as R´-N=N-R, where R´ is a heterocyclic group, R is a coupling component (including heterocyclic group Minute). According to the different structures, pyridylazo, thiazolylazo, and benzothiazolylazo reagents are most widely used in analysis and detection. These three types of reagents have been widely used in the metal ion Ni 2+ 、Co 2+ , Zn 2+ , Pd 2+ , Hg 2+ 、Ag + 、Cu 2+ Photometric analysis and detection of metal ions (theoretical test - chemistry volume, Zhang Hanpeng, 1996, 32 (1): 53-58). Thiazole azo reagents have attracted widespread attention because of their easy synthesis and good selectivity. B...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D513/04G01N21/78
CPCC07D513/04G01N21/78
Inventor 尚建鹏许琳刘文王尚芝樊月琴解海孟双明
Owner SHANXI DATONG UNIV
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