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Synthesis method of methyl picolinate

A technology of methyl picolinate and a synthesis method, which is applied in the field of electrochemical organic synthesis, and achieves the effects of cheap and easily available raw materials, reduced air pollution and low cost

Inactive Publication Date: 2017-11-28
LIAOCHENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] So far, there are no studies and reports on the electrochemical reduction of 2-bromopyridine in a carbon dioxide atmosphere

Method used

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  • Synthesis method of methyl picolinate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1 A kind of synthetic method of methyl 2-pyridinecarboxylate, concrete steps are as follows:

[0019] a. Preparation of electrolyte

[0020] Mix 1 mmol (95 ul) 2-bromopyridine with 1 mmol (0.2102 g) tetraethylammonium bromide and 0.129 mol (10 mL) N, N -Dimethylformamide is mixed into an electrolyte, and then placed in a one-chamber electrolytic cell with silver as the cathode and magnesium rod as the anode, 2-bromopyridine, tetraethylammonium bromide and N,N -Dimethylformamide is analytically pure, wherein: 2-bromopyridine is a substrate, N,N -Dimethylformamide is the solvent after 4Å grade molecular sieve drying, and tetraethylammonium bromide is the supporting electrolyte;

[0021] b. Electrocarboxylation reaction

[0022] Under normal pressure, carbon dioxide was introduced into the above electrolytic cell for 30 min, and then at 8 mA / cm 2 Electrolyze at a constant current density of 2.0 F per mole of 2-bromopyridine, and F is the Faraday constant; ...

Embodiment 2

[0029] Embodiment 2 A kind of synthetic method of methyl 2-pyridinecarboxylate, concrete steps are as follows:

[0030] a. Preparation of electrolyte

[0031] Mix 1 mmol (95 ul) 2-bromopyridine with 1 mmol (0.3224 g) tetrabutylammonium bromide and 0.129 mol (10 mL) N,N -Dimethylformamide is mixed into an electrolyte, and then placed in a one-chamber electrolytic cell with a silver sheet as a cathode and a magnesium rod as an anode, 2-bromopyridine, tetrabutylammonium bromide and N,N -Dimethylformamide is analytically pure, wherein: 2-bromopyridine is a substrate, N,N -Dimethylformamide is the solvent after 4Å grade molecular sieve drying, and tetrabutylammonium bromide is the supporting electrolyte;

[0032] b. Electrocarboxylation reaction

[0033] Under normal pressure, carbon dioxide was introduced into the above electrolytic cell for 30 min, and then at 8 mA / cm 2 Electrolyze at a constant current density of 2.0 F per mole of 2-bromopyridine, and F is the Faraday consta...

Embodiment 3

[0040] Embodiment 3 A kind of synthetic method of methyl 2-pyridinecarboxylate, concrete steps are as follows:

[0041] Mix 1 mmol (95 ul) 2-bromopyridine with 1 mmol (0.3224 g) tetrabutylammonium bromide and 0.129 mol (10 mL) N,N -Dimethylformamide is mixed into an electrolyte, and then placed in a one-chamber electrolytic cell with nickel as the cathode and magnesium rod as the anode, 2-bromopyridine, tetrabutylammonium bromide and N,N -Dimethylformamide is analytically pure, wherein: 2-bromopyridine is a substrate, N,N -Dimethylformamide is the solvent after 4Å grade molecular sieve drying, and tetrabutylammonium bromide is the supporting electrolyte;

[0042] b. Electrocarboxylation reaction

[0043] Under normal pressure, carbon dioxide was introduced into the above electrolytic cell for 30 min, and then at 8 mA / cm 2 Electrolyze at a constant current density of 2.0 F per mole of 2-bromopyridine, and F is the Faraday constant;

[0044] c. Esterification reaction

[00...

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Abstract

The invention discloses a synthesis method of methyl picolinate. The method comprises the following steps that 2-bromopyridine, 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 are mixed into an electrolyte; carbon dioxide is introduced for 30min at normal pressure; then, electric carboxylation reaction is performed by using constant current (the carbon dioxide is continuously introduced in the electrolysis process until the electrolysis is completed); then, the methyl picolinate is obtained through esterification and post treatment. A reaction system is simple; the control is easy; in addition, rich Cl resources and CO2 are used as one of raw materials; the raw materials are cheap and can be easily obtained; the cost is low; a novel path is developed for the study on challenging organic matters of green synthetic heterocyclic ring carboxylic acid derivatives and the like.

Description

technical field [0001] The invention relates to the technical field of electrochemical organic synthesis, in particular to a method for synthesizing methyl 2-picolinate. Background technique [0002] Carbon dioxide is a major greenhouse gas, and it is of great significance to fix and utilize it. In recent years, the electrocarboxylation reaction to activate and fix carbon dioxide as a variety of economically competitive chemicals by electrochemical methods has attracted more and more attention. One of the most efficient ways to use substances. In the last few decades, studies on the electrocarboxylation of halides have been reported. Cobalt, nickel, palladium and other complexes as catalysts can effectively improve the yield of the corresponding reduction products of organic halides. [0003] Methyl 2-pyridinecarboxylate is an important fine chemical, pharmaceutical and material intermediate. Singh et al. in S.K.Singh, M.S. Reddy, M. Mangle, K.R. Ganesh, Tetrahedron 63 (...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/00
CPCC25B3/00
Inventor 陈宝丽张英天罗佩佩于淑娴高翠张宪玺周华伟曲孔岗
Owner LIAOCHENG UNIV
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