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Preparation method of 2-amino-3-nitro pyridine

A technology of nitropyridine and aminopyridine, applied in the field of preparation of 2-amino-3-nitropyridine, can solve the problems of affecting the reaction, difficult separation, low yield and the like, and achieves less by-products, high yield, The effect of a simple synthesis process

Inactive Publication Date: 2014-03-26
常熟市联创化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional method of synthesizing 2-amino-3-nitropyridine has a low yield and produces a large number of by-products, which are not easy to separate and will affect subsequent reactions

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Provide a kind of preparation method of 2-amino-3-nitropyridine, comprising the steps of:

[0014] (1) Dissolve 2-aminopyridine in dimethylformamide and stir, add liquid bromine dropwise to the reaction solution at a rate of one drop per 4 seconds, heat and react at 50°C for 2 hours and then process to obtain 2-aminopyridine -5-bromopyridine;

[0015] (2) Slowly add a mixture of concentrated nitric acid and concentrated sulfuric acid dropwise to the 2-amino-5-bromopyridine obtained in step (1). After the dropwise addition, raise the temperature of the reaction solution to 114°C and react for 6 hours. Hydrogenation reduction gives 2-amino-3-nitropyridine.

Embodiment 2

[0017] Provide a kind of preparation method of 2-amino-3-nitropyridine, comprising the steps of:

[0018] (1) Dissolve 2-aminopyridine in dichloromethane and stir, add liquid bromine dropwise to the reaction solution at a rate of one drop every 3 seconds, heat and react at 58°C for 1.5 hours and then process to obtain 2-amino-5 - Bromopyridine;

[0019] (2) Slowly add the mixture of concentrated nitric acid and concentrated sulfuric acid dropwise to the 2-amino-5-bromopyridine obtained in step (1). After the dropwise addition, raise the temperature of the reaction solution to 118°C and react for 6.5 hours. Hydrogenation reduction gives 2-amino-3-nitropyridine.

Embodiment 3

[0021] Provide a kind of preparation method of 2-amino-3-nitropyridine, comprising the steps of:

[0022] (1) Dissolve 2-aminopyridine in ethanol and stir, add liquid bromine dropwise to the reaction solution at a rate of one drop every 5 seconds, heat and react at 53°C for 1 hour and then process to obtain 2-amino-5-bromo pyridine;

[0023] (2) Slowly add the mixture of concentrated nitric acid and concentrated sulfuric acid dropwise to the 2-amino-5-bromopyridine obtained in step (1). After the dropwise addition, raise the temperature of the reaction solution to 110°C and react for 7 hours. Hydrogenation reduction gives 2-amino-3-nitropyridine.

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PUM

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Abstract

The invention discloses a preparation method of 2-amino-3-nitro pyridine. The method comprises the following steps: dissolving 2-aminopyridine in an organic solvent and stirring, dropwise adding liquid bromine into the reaction solution with a speed of 3-5 s / drop, heating for reaction for a certain time and treating to obtain 2-amino-5-pyridyl bromide; slowly dropwise adding a nitrating agent into the 2-amino-5-pyridyl bromide obtained in the step (1), after the addition, heating the reaction liquid to 110-120 DEG C, reacting for 6-7 h, and carrying out posttreatment and hydrogenation reduction to obtain the 2-amino-3-nitro pyridine. By the above way, the preparation method of 2-amino-3-nitro pyridine provided by the invention has simple process and high yield. The obtained 2-amino-3-nitro pyridine has a small amount of by-products and high purity, the product can be obtained by simple posttreatment, and a next step of reaction can be carried out directly. The method greatly reduces production cost and is applicable for mass production.

Description

technical field [0001] The invention relates to the field of fine organic synthesis, in particular to a preparation method of 2-amino-3-nitropyridine. Background technique [0002] Pyridine and its derivatives are a very important class of fine chemical products with a wide range of uses, especially in the fields of medicine and pesticides. Among pesticides, the herbicide paraquat is used in the largest amount, and niacin and niacinamide are used in the largest amount in medicine and animal feed. There are many kinds of pyridine special fine chemicals, some of which have high added value, and pyridine derivatives are widely used and have great development potential. The molecular formula of 2-amino-3-nitropyridine is C 5 h 5 N 3 o 2 , with a molecular weight of 139.11, can be used to synthesize 3-amino-2-fluoropyridine, 2-fluoro-3-nitropyridine and 2,3-diaminopyridine. The traditional method for synthesizing 2-amino-3-nitropyridine has a low yield and produces a large ...

Claims

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Application Information

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IPC IPC(8): C07D213/73
CPCC07D213/73
Inventor 陈雪平
Owner 常熟市联创化学有限公司
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