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Preparation method of aminopyridine chloride

A technology of aminopyridine and chloride, which is applied in the field of preparation of aminopyridine chloride, can solve the problems of many by-products in the product, complex operation process, and low product yield, and achieve less by-products, high product purity, and post-treatment simple effect

Inactive Publication Date: 2012-02-22
HARBIN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The present invention aims to solve the problems of low product yield, many by-products in the product, complex operation process and serious environmental pollution existing in the existing aminopyridine synthesis process, and provides a preparation method of aminopyridine chloride

Method used

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  • Preparation method of aminopyridine chloride
  • Preparation method of aminopyridine chloride
  • Preparation method of aminopyridine chloride

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specific Embodiment approach 1

[0012] Specific embodiment one: the preparation method of a kind of aminopyridine chloride of this embodiment, specifically is finished according to the following steps:

[0013] 1. Electrolysis: Dissolve aminopyridine in the hydrochloric acid solution of the electrolytic cell without diaphragm to obtain the electrolytic solution of aminopyridine, then turn on the power supply, and at the same time pass nitrogen gas above the electrolytic cell without diaphragm to adjust the current intensity to 0.1A~0.4A , the voltage is 1.1V ~ 1.4V, electrolytic chlorination at room temperature for 2 ~ 12h, to obtain the reaction solution after electrolysis; 2. Separation and purification: add alkaline substances to the reaction solution after electrolysis in step 1 to adjust the pH value to 8 ~9, then use organic solvent extraction, separate the extraction phase, use the mass fraction of 15% ~ 35% sodium chloride solution to wash the extraction phase, until the pH value of the extraction pha...

specific Embodiment approach 2

[0025] Embodiment 2: The difference between this embodiment and Embodiment 1 is that the mass fraction of HCl in the hydrochloric acid solution described in step 1 is 15-30%. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0026] Embodiment 3: The difference between this embodiment and Embodiment 1 or 2 is that the mass fraction of HCl in the hydrochloric acid solution described in step 1 is 20%. Others are the same as in the first or second embodiment.

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Abstract

The invention discloses a preparation method of an aminopyridine chloride, relating to the field of preparation of the aminopyridine chloride and aiming to solve the problems of low product yield, more byproducts in products, complex operation process and serious environment pollution in the traditional aminopyridine synthesis process. The preparation method comprises the following steps of: 1, electrolyzing, and 2, separating and purifying. The preparation method disclosed by the invention has the advantage of: 1, very high selectivity, fewer byproducts in the products, high product purity and simplicity for postprocessing; 2, simplicity for operation, no need of any catalysts, mild reaction conditions and low energy consumption; 3, reduced consumed energy for reaction due to adoption of a diaphragm-free electrolytic cell; 4, capability of meeting requirements of green chemistry for environment friendliness; and 5, production safety. The preparation method disclosed by the invention is mainly used for preparing 2-amino-5-chloropyridine and 3-amino-2-chloropyridine.

Description

technical field [0001] The invention relates to the field of preparation of aminopyridine chloride. Background technique [0002] Aminopyridine chloride is an important pharmaceutical and pesticide intermediate, mainly used in the synthesis of important chemical products such as pharmaceuticals, pesticides, and dyes. Such as 3-amino-2-chloropyridine and its derivatives are a class of very useful aminopyridine derivatives, which can be used as an important pharmaceutical intermediate to synthesize the drug-pirenzepine for the treatment of digestive system diseases, pirenzepine is An excellent anti-ulcer drug, mainly used in the treatment of gastric and duodenal ulcers. 2,3-dichloropyridine synthesized from 3-amino-2-chloropyridine is an important intermediate in the synthesis of anthranilamide pesticides (such as chlorantraniliprole and cyantraniliprole developed by DuPont). Other aminopyridine chlorides can be used to prepare important intermediates of painkillers, anti-in...

Claims

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Application Information

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IPC IPC(8): C25B3/06
Inventor 刘波王慧娟由君于晓晶秦伟艳
Owner HARBIN UNIV OF SCI & TECH
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