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Novel synthesis process of 2,2'-dipyridyl

A bipyridine and new process technology, which is applied in the new process field of 2,2'-bipyridine synthesis, can solve the problems that cannot meet the production requirements, are not suitable for recycling, and the catalyst life is short, so as to achieve low production cost and environmental protection. Friendly, high reaction yield effect

Active Publication Date: 2013-06-26
NANJING COSTAR BIOTECHNOLOGY RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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
Effect test

Embodiment 1

[0018] Embodiment 1: The new technique of 2,2'-bipyridine synthesis comprises the following steps:

[0019] (1) Coupling: 125kg of 2-chloropyridine, 250kg of solvent DMAC, 70kg of catalyst triphenylphosphine, 60kg of zinc powder, and 5kg of nickel chloride were added to the reaction kettle in sequence, and the temperature was raised to 60°C for 2 hours, and the sample was analyzed;

[0020] (2) Precipitation: Step (1) After sampling and analysis, when the content of 2-chloropyridine is <0.5%, the reaction ends, the temperature is controlled at 100°C, and the solvent DMAC is removed under reduced pressure;

[0021] (3) Alkaline hydrolysis: Add 900kg of 20% ammonia water and 150kg of ammonium sulfate to the solid obtained in step (2) and heat up to 40°C for alkaline hydrolysis for 4 hours, then add 900kg of toluene, and press filter to obtain the filtrate;

[0022] (4) Extraction: After the alkali hydrolysis in step (3) is hydraulically filtered, the filtrate is subjected to liq...

Embodiment 2

[0026] Embodiment 2: The new technique of 2,2'-bipyridine synthesis comprises the following steps:

[0027] (1) Coupling: 125kg of 2-chloropyridine, 275kg of solvent DMAC, 70kg of catalyst triphenylphosphine, 65kg of zinc powder, and 7kg of nickel chloride were added to the reaction kettle in sequence, and the temperature was raised to 70°C for 2 hours, and sampling and analysis were performed;

[0028] (2) Precipitation: Step (1) After sampling and analysis, when the content of 2-chloropyridine is <0.5%, the reaction ends, the temperature is controlled at 110°C, and the solvent DMAC is removed under reduced pressure;

[0029] (3) Alkaline hydrolysis: Add 925kg of 20% ammonia water and 175kg of ammonium sulfate to the solid obtained in step (2) and raise the temperature to 50°C for alkaline hydrolysis for 4 hours, then add 950kg of toluene, and press filter to obtain the filtrate;

[0030] (4) Extraction: After the alkali hydrolysis in step (3) is hydraulically filtered, the f...

Embodiment 3

[0034] Embodiment 3: The new technique of 2,2'-bipyridine synthesis comprises the following steps:

[0035] (1) Coupling: 130kg of 2-chloropyridine, 300kg of solvent DMAC, 75kg of catalyst triphenylphosphine, 65kg of zinc powder, and 8kg of nickel chloride were added to the reaction kettle in sequence, and the temperature was raised to 90°C for 3 hours, and the sample was analyzed;

[0036] (2) Precipitation: Step (1) After sampling and analysis, when the content of 2-chloropyridine is <0.5%, the reaction ends, the temperature is controlled at 120°C, and the solvent DMAC is removed under reduced pressure;

[0037] (3) Alkaline hydrolysis: Add 975kg of 20% ammonia water and 225kg of ammonium sulfate to the solid obtained in step (2) and raise the temperature to 60°C for alkaline hydrolysis for 5 hours, then add 950kg of toluene, and press filter to obtain the filtrate;

[0038] (4) Extraction: After the alkali hydrolysis in step (3) is hydraulically filtered, the filtrate is su...

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PUM

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Abstract

The invention discloses a novel synthesis process of 2,2'-dipyridyl. The novel synthesis process adopting 2-chloropyridine as the raw material comprises the following steps of: coupling the material to obtain 2,2'-dipyridyl under the catalytic action of the catalyst; screening out a better alkaline hydrolysis reagent and auxiliaries to carry out alkaline hydrolysis by selecting an alkaline hydrolysis reagent and auxiliaries; and obtaining refined 2,2'-dipyridyl through the steps including extracting, acid-washing and re-alkaline hydrolyzing and the like. The novel synthesis process disclosed by the invention is simple, capable of greatly reducing the production cost, capable of reducing the reaction yield and capable of optimizing the process flow.

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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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/22C07D213/127
Inventor 李健葛九敢王红明黎广薛谊
Owner NANJING COSTAR BIOTECHNOLOGY RES INST CO LTD
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