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Synthesis method of 2,2'-dipyridyl

A synthesis method and bipyridine technology, applied in the direction of organic chemistry and the like, can solve the problems of unsuitable recycling, short catalyst life, unable to meet production requirements, etc., and achieve the effects of low production cost, high reaction yield and environmental friendliness.

Inactive Publication Date: 2013-04-10
ANHUI COSTAR BIOCHEM CO LTD
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  • Abstract
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AI Technical Summary

Problems solved by technology

The catalyst life of this method is short, it is not suitable for recycling, and it cannot meet the requirements of production.

Method used

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Examples

Experimental program
Comparison scheme
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Embodiment Construction

[0019] A kind of synthetic method of 2,2'-bipyridine, concrete steps are:

[0020] (1) Coupling: Add 2-chloropyridine, solvent DMAC, catalyst triphenylphosphine, zinc powder, nickel chloride, dodecyl dimethyl betaine into the reaction kettle in sequence, and heat up to 60-70°C. Insulation reaction for 3 hours, and then sampling analysis, wherein the mass ratio of 2-chloropyridine: solvent DMAC: catalyst triphenylphosphine: zinc powder: nickel chloride, dodecyl dimethyl betaine = 125: 300: 70: 60:5:3;

[0021] (2) Precipitation: Step (1) After sampling and analysis, when the content of 2-chloropyridine is less than 0.5%, the reaction is over, the temperature is controlled at 100-130°C, the solvent DMAC is removed under reduced pressure, and the solid substance is obtained by filtration;

[0022] (3) Alkaline hydrolysis: Add 10-12% sodium hydroxide solution and ammonium bicarbonate to the solid matter obtained in step (2) and heat up to 65-70°C, and perform alkaline hydrolysis ...

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PUM

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Abstract

The invention discloses a synthesis method of 2,2'-dipyridyl, mainly comprising the following steps of: coupling 2-chloropyridine as a raw material under the catalysis effect of a catalyst to obtain 2,2'-dipyridyl; screening an alkaline hydrolysis reagent and an auxiliary agent, which have the better advantage, by selecting the alkaline hydrolysis reagent and the auxiliary agent, to carry out alkaline hydrolysis; and finally, carrying out steps of extraction, acid washing, second time of alkaline hydrolysis, second time of acid washing, alkaline hydrolysis and the like to obtain refined 2,2'-dipyridyl. The method disclosed by the invention is simple; the production cost is greatly reduced and the reaction yield is improved; and meanwhile, a process flow is further optimized.

Description

technical field [0001] The invention belongs to the fields of chemical industry and pesticide, and in particular relates to a new process for synthesizing 2,2'-bipyridine. Background technique [0002] 2,2'-bipyridine is one of the isomers of bipyridine, and is an important organic synthesis intermediate, mainly used in pharmaceutical intermediates, organic synthesis, etc. At the same time, it is also a widely used chelating agent and coating additive, widely used in the production of dyes, pesticides and spices. Therefore, it will be of great significance to study its synthesis and industrialization. [0003] The traditional method of synthesizing 2,2'-bipyridine is to use Raney nickel as catalyst and pyridine as raw material. The catalyst life of this method is short, it is not suitable for recycling, and it cannot meet the requirements of production. [0004] Using dihalopyridine as raw material and using composite catalyst to synthesize 2,2'-bipyridine has become the ...

Claims

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Application Information

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IPC IPC(8): C07D213/22C07D213/127
Inventor 王红明葛九敢俞建良刘善和
Owner ANHUI COSTAR BIOCHEM CO LTD
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