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Synthetic method of thiazole-4-formic acid

A synthesis method, the technology of formic acid, applied in the field of electrochemical organic synthesis, can solve the problems of harsh conditions, cumbersome steps, long reaction time, etc., and achieve the effects of easy process control, simple system and high use value

Active Publication Date: 2018-12-11
LIAOCHENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method has long reaction time, harsh conditions and complicated steps

Method used

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  • Synthetic method of thiazole-4-formic acid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1 A kind of synthetic method of thiazole-4-carboxylic acid, concrete steps are as follows:

[0024] a. Preparation of electrolyte

[0025] Mix 1mmol (89μL) of 4-bromothiazole with 1mmol (0.1657g) of tetraethylammonium chloride and 0.129mol (10mL) of N,N-dimethylformamide to form an electrolyte, then put titanium as the cathode and magnesium In a one-chamber electrolytic cell with the rod as the anode, 4-bromothiazole, tetraethylammonium chloride and N,N-dimethylformamide are analytically pure, of which: 4-bromothiazole is the substrate, N,N-di Methylformamide is Grade molecular sieve dried solvent, tetraethylammonium chloride as supporting electrolyte.

[0026] b. Electrocarboxylation reaction

[0027] Under normal pressure, carbon dioxide was passed into the above electrolytic cell for 30 minutes, and then at 3mA / cm 2 The constant current density is electrolyzed (the electrolysis process is fed into carbon dioxide until the end of the electrolysis), the...

Embodiment 2

[0032] Embodiment 2 A kind of synthetic method of thiazole-4-carboxylic acid, concrete steps are as follows:

[0033] a. Preparation of electrolyte

[0034] Mix 1mmol (89μL) of 4-bromothiazole with 1mmol (0.2572g) of tetrabutylammonium iodide and 0.129mol (10mL) of N,N-dimethylformamide to form an electrolyte, then put copper as the cathode and magnesium In a one-chamber electrolytic cell with the rod as the anode, 4-bromothiazole, tetrabutylammonium iodide and N,N-dimethylformamide are analytically pure, of which: 4-bromothiazole is the substrate, N,N-di Methylformamide is Grade molecular sieve dried solvent, tetrabutylammonium iodide as supporting electrolyte.

[0035] b. Electrocarboxylation reaction

[0036] Under normal pressure, pass carbon dioxide into the electrolytic cell for 30 minutes, and then use 1mA / cm 2 The constant current density is electrolyzed (the electrolysis process has been passed into carbon dioxide until the end of the electrolysis), the current f...

Embodiment 3

[0041] Embodiment 3 A kind of synthetic method of thiazole-4-carboxylic acid, concrete steps are as follows:

[0042] a. Preparation of electrolyte

[0043] Mix 1mmol (89μL) of 4-bromothiazole with 1mmol (0.2171g) of tetraethylammonium tetrafluoroborate and 0.129mol (10mL) of N,N-dimethylformamide to form an electrolyte, and then put it into the electrolyte with stainless steel as the cathode and In a one-chamber electrolytic cell with a magnesium rod as the anode, 4-bromothiazole, tetraethylammonium tetrafluoroborate and N,N-dimethylformamide are analytically pure, of which: 4-bromothiazole is the substrate, N,N -Dimethylformamide is Grade molecular sieve dried solvent, tetraethylammonium tetrafluoroborate as supporting electrolyte.

[0044] b. Electrocarboxylation reaction

[0045] Under normal pressure, carbon dioxide was passed into the above electrolytic cell for 30 minutes, and then at 9mA / cm 2 The constant current density is electrolyzed (the electrolysis process is...

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Abstract

The invention discloses a synthetic method of thiazole-4-formic acid. The method comprises the steps that 4-bromo-thiazole is added into a quaternary ammonium salt solution to prepare electrolyte, theconstant current is connected into the electrolyte to conduct an electric carboxylation reaction in the atmosphere of carbon dioxide, an acetonitrile water solution is adopted to conduct hydrolysis,and thiazole-4-formic acid can be obtained, wherein quaternary ammonium salt is selected from tetraethylammonium chloride hydrate, tetraethylammonium bromide, tetraethylammonium iodide, tetraethyl tetrafluoroborate, tetrabutylammonium chloride hydrate, tetrabutylammonium bromide and tetrabutylammonium iodide, the solvent of the electrolyte is N,N-dimethyl formamide or acetonitrile. The reaction system of the synthetic method is simple, the condition is moderate, the process is easy to control, carbon dioxide can be utilized, and a route is provided for solution of greenhouse effect gas.

Description

technical field [0001] The invention relates to the technical field of electrochemical organic synthesis, in particular to a synthesis method of thiazole-4-carboxylic acid. Background technique [0002] Thiazole-4-carboxylic acid, also known as 4-thiazolecarboxylic acid, is an important intermediate for the synthesis of thiabendazole, a very important pharmaceutical, pesticide intermediate and organic synthesis reagent, and has a wide range of uses. The traditional method for synthesizing thiazole-4-carboxylic acid is to add formamide dropwise to P 2 S 5 Dispersed in ethylene glycol dimethyl ether solvent to obtain thioformamide (HCSNH 2 ), then react with methyl bromopyruvate to obtain methyl thiazole-4-carboxylate, and further hydrolyze to obtain the product. This method requires strict control of reaction temperature, longer reaction time, harsh and cumbersome conditions, more serious pollution, and lower reaction yield. The synthesis process reported by Qiu Tao et al...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/00G01N30/02
CPCC25B3/00G01N30/02
Inventor 陈宝丽张英天宋鹏飞高翠于淑娴薛淑洁张梦琦皮琳琳
Owner LIAOCHENG UNIV
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