One-step method for preparing 3-aminopyridine

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 ...

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