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Synthetic method of isonicotinic acid

A synthetic method and technology of isonicotinic acid, applied in the direction of electrolysis process, electrolysis components, electrolysis organic production, etc., can solve the problems of inconvenient product purification, achieve the effects of reducing air pollution, convenient operation, and good application prospects

Inactive Publication Date: 2017-11-17
LIAOCHENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalyst Schiff base is used in this method, which brings inconvenience to product purification.
[0004] So far, there are no studies and reports on the electrocarboxylation of 4-bromopyridine to fix CO2 to synthesize isonicotinic acid

Method used

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  • Synthetic method of isonicotinic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1 A method for synthesizing isonicotinic acid, the specific steps are as follows:

[0018] a. Preparation of electrolyte

[0019] Combine 1mmol (96ul) 4-bromopyridine with 1 mmol (0.2171g) tetraethylammonium tetrafluoroborate and 0.129 mol (10 mL) N,N -Dimethylformamide is mixed to form an electrolyte, and then placed in a one-chamber electrolytic cell with stainless steel as the cathode and magnesium rod as the anode, 4-bromopyridine, tetraethylammonium tetrafluoroborate and N,N -Dimethylformamide is analytically pure, of which: 4-bromopyridine is the substrate, N, N -Dimethylformamide is the dried solvent of 4Å grade molecular sieve, and tetraethylammonium tetrafluoroborate is the supporting electrolyte;

[0020] b. Electrocarboxylation reaction

[0021] Under normal pressure, inject carbon dioxide into the above electrolytic cell for 30 minutes, and then use 8 mA / cm 2 Conduct electrolysis at a constant current density of (the electrolysis process has been fed with c...

Embodiment 2

[0026] Example 2 A method for synthesizing isonicotinic acid, the specific steps are as follows:

[0027] a. Preparation of electrolyte

[0028] Combine 1mmol (96ul) 4-bromopyridine with 1 mmol (0.1657g) tetraethylammonium chloride and 0.129 mol (10 mL) N, N -Dimethylformamide is mixed to form an electrolyte, and then placed in a one-compartment electrolytic cell with a platinum plate as the cathode and a magnesium rod as the anode, 4-bromopyridine, tetraethylammonium chloride and N,N -Dimethylformamide is analytically pure, of which: 4-bromopyridine is the substrate, N,N -Dimethylformamide is the dried solvent of 4Å grade molecular sieve, and tetraethylammonium chloride is the supporting electrolyte;

[0029] b. Electrocarboxylation reaction

[0030] Under normal pressure, inject carbon dioxide into the above electrolytic cell for 30 minutes, and then use 8 mA / cm 2 Electrolysis is carried out at a constant current density of (the electrolysis process has been filled with carbon diox...

Embodiment 3

[0035] Example 3 A method for synthesizing isonicotinic acid, the specific steps are as follows:

[0036] Combine 1mmol (96ul) 4-bromopyridine with 1 mmol (0.3694 g) tetrabutylammonium iodide and 0.129 mol (10 mL) N, N -Dimethylformamide is mixed to form an electrolyte, and then placed in a one-chamber electrolytic cell with silver as the cathode and magnesium rod as the anode, 4-bromopyridine, tetrabutylammonium iodide and N,N -Dimethylformamide is analytically pure, of which: 4-bromopyridine is the substrate, N,N -Dimethylformamide is the dried solvent of 4Å grade molecular sieve, and tetrabutylammonium iodide is the supporting electrolyte;

[0037] b. Electrocarboxylation reaction

[0038] Under normal pressure, inject carbon dioxide into the above electrolytic cell for 30 minutes, and then use 4 mA / cm 2 Electrolysis is carried out at a constant current density of (the electrolysis process is filled with carbon dioxide until the end of the electrolysis), the energization amount i...

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Abstract

The invention discloses a synthetic method of isonicotinic acid. The method comprises the following steps: mixing 4-bromopyridine with N, N-dimethylformamide or acetonitrile and tetraethylammonium chloride or tetraethylammonium bromide or tetraethylammonium iodide or tetraethylammonium tetrafluoroborate or tetrabutylammonium chloride or tetrabutylammonium bromide or tetrabutylammonium iodide to form an electrolyte; introducing carbon dioxide at normal pressure for 30 minutes; and carrying out electrolysis at a constant current, keeping introducing the carbon dioxide during the electrolysis process until the electrolysis is ended, and obtaining the isonicotinic acid after carrying out post-treatments. According to the synthetic method of the isonicotinic acid, the reaction system is simple and easy to control, the rich C1 resource, namely the carbon dioxide is used as one of the raw materials, is cheap and easy to obtain, is low in cost and does not pollute the environment, and therefore a new way is developed for the study of the green isonicotinic acid, an extremely good application prospect of the synthetic method is displayed in the medicine industry, the food industry, the chemical industry and the electronic industry, and the synthetic method of the isonicotinic acid is a process route with high industrial synthetic value.

Description

Technical field [0001] The invention relates to the technical field of electrochemical organic synthesis, in particular to a method for synthesizing isonicotinic acid. Background technique [0002] Isonicotinic acid, also known as 4-picolinic acid, is an important intermediate for the synthesis of anti-tuberculosis drug Remifen. It can also be used as an anti-corrosion agent, electroplating additive, non-ferrous metal flotation agent, polyvinyl chloride heat stabilizer and photosensitive resin stabilizer Body etc. Traditional methods for synthesizing isonicotinic acid include potassium permanganate oxidation, ozone oxidation, catalytic air oxidation, and nitric acid oxidation. However, the above-mentioned methods generally have problems such as complex process, environmental pollution, and serious peroxide. Because electrochemical synthesis has the advantages of high reaction selectivity, short process flow, mild reaction conditions and low pollution, people pay great attention...

Claims

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Application Information

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IPC IPC(8): C25B3/00
CPCC25B3/00
Inventor 陈宝丽张英天罗佩佩张宪玺周华伟曲孔岗
Owner LIAOCHENG UNIV
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