One-step method for preparing 3-aminopyridine

A technology of aminopyridine and cyanopyridine, applied in the field of one-step preparation of 3-aminopyridine, can solve problems such as poor energy saving effect, and achieve the possible effects of saving energy, saving production costs and reducing side reactions

Inactive Publication Date: 2018-04-27
CANGZHOU LINGANG YANUO CHEM CO LTD
View PDF2 Cites 6 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In terms of pesticides, it is used as a raw material for fungicide Butiobate; 3-aminopyridine is an important pharmaceutical, pesticide, and fine chemical intermediate, and its downstream product 2,3-dichloropyridine is an important raw material for the synthesis of insecticide Kangkuan. The synthesis method is mainly obtained by the following (1) using 3-bromopyridine as raw material, reacting with concentrated ammonia water under heating in the presence of copper sulfate; (2) using 3-cyanopyridine as raw material, under mild conditions Hydrolysis to generate nicotinamide, which is obtained by Hofman degradation reaction; taking the second method as an example, 3-cyanopyridine must first be catalyzed by alkali to obtain nicotinamide or be separated or not, and then Hofman Degradation reaction can obtain 3-aminopyridine; It is found in the implementation of its preparation method that its energy-saving effect is relatively poor

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In the 2000L four-necked glass reaction flask, add 923g of available chlorine successively as 10% sodium hypochlorite (1.3mol) solution, 300g water and 200g30% (1.5mol) sodium hydroxide solution, and cool to 0°C while stirring under the ice-salt bath; Grind 104g (1mol) of 3-cyanopyridine in a mortar, add it into a stirring four-necked reaction bottle through a paper feeding tube, rinse the mortar and the 3-cyanopyridine adhering to the glass port with a washing bottle And add it in a four-necked reaction flask, the temperature will rise during the addition process, keep the ice-salt bath and control the addition speed of 3-cyanopyridine so that the temperature of the liquid in the reaction flask does not exceed 5°C. After adding the 3-cyanopyridine powder, remove the ice-salt bath to allow the reaction system to return to temperature, and use the ice-salt bath to control the temperature of the reaction system not to exceed 25°C. After about 3 to 6 hours, the reaction sol...

Embodiment 2

[0023] In the 2000L four-necked glass reaction flask, add 817g of available chlorine successively as a 10% sodium hypochlorite (1.15mol) solution and 300g of water, and cool to 0°C while stirring under an ice salt bath; get 104g (1mol) of 3-cyanopyridine in the Grind finely in the mortar, add it into the stirring four-necked reaction flask through the paper feeding tube, rinse the mortar with the washing bottle and add the 3-cyanopyridine adhered to the glass mouth into the four-necked reaction flask together, the adding process The medium temperature will rise sharply, keep the ice-salt bath and make the liquid temperature in the reaction bottle not exceed 5°C by controlling the addition rate of 3-cyanopyridine. After the 3-cyanopyridine powder is added, 200g of 30% (1.5mol) sodium hydroxide solution is added in the dropping tube, and the liquid caustic soda solution is added dropwise to the four-necked reaction bottle while stirring, as the liquid caustic soda solution is add...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention relates to a one-step method for preparing 3-aminopyridine. Hofmann degradation is directly performed when 3-cyanopyridine is not hydrolyzed into nicotinamide, the reaction time of a reaction device is shortened, reaction steps are decreased, application of energy is decreased, and energy is saved. The method includes the steps: 1) preparing raw materials such as sodium hypochloritesolution with available chlorine of 10%, water, sodium hydroxide solution and 3-cyanopyridine; 2) sequentially placing the sodium hypochlorite solution, the water and the sodium hydroxide solution into a four-port glass reaction bottle, stirring mixture under ice-salt bath, and cooling the mixture to reach the temperature of 0 DEG C; 3) taking 3-cyanopyridine, placing the taken 3-cyanopyridine into a mortar, grinding the 3-cyanopyridine, adding the grinded 3-cyanopyridine into the stirring four-port reaction bottle by a paper adding cylinder, flushing the mortar by the aid of a washing bottleand the 3-cyanopyridine adhered on the glass ports, adding residues into the four-port reaction bottle, heating mixture in the adding process, keeping the ice-salt bath, controlling the adding speed of the 3-cyanopyridine, and enabling the temperature of liquid in the reaction bottle not to exceed 5 DEG C.

Description

technical field [0001] The invention relates to a method for preparing 3-aminopyridine in one step. Background technique [0002] As we all know, 3-aminopyridine is a chemical substance with a molecular formula of C5H6N2, which is used in medicine as an intermediate for the production of gastric ulcer and duodenal ulcer drugs. In terms of pesticides, it is used as a raw material for fungicide Butiobate; 3-aminopyridine is an important pharmaceutical, pesticide, and fine chemical intermediate, and its downstream product 2,3-dichloropyridine is an important raw material for the synthesis of insecticide Kangkuan. The synthesis method is mainly obtained by the following (1) using 3-bromopyridine as raw material, reacting with concentrated ammonia water under heating in the presence of copper sulfate; (2) using 3-cyanopyridine as raw material, under mild conditions Hydrolysis to generate nicotinamide, which is obtained by Hofman degradation reaction; taking the second method as ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/73
CPCC07D213/73
Inventor 凌广轩刘晓民温宁李永辉郑忠峰彭德彪王鹏浩郑少坡高寿松相聪史洪波
Owner CANGZHOU LINGANG YANUO CHEM CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap