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Preparation method of 3-hydroxy-2-nitropyridine

A technology of nitropyridine and hydroxypyridine, which is applied in the field of preparation of 3-hydroxy-2-nitropyridine, can solve the problems of long reaction time and easy danger, and achieve the effects of energy saving, risk reduction and high purity

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 reaction time in the synthesis process of traditional 3-hydroxy-2-nitropyridine is long, sometimes even one day, which is prone to danger

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0014] (1) Add concentrated sulfuric acid to 3-hydroxypyridine while stirring, and volatilize hydrogen chloride under reduced pressure, then add oleum and fuming nitric acid with a mass percentage of 42%, heat up to 80°C and stir for 3 hours, get the mixture;

[0015] (2) Add concentrated ammonia water dropwise to the mixture, adjust the pH value to make the pH value 5.5, then add water and stir to obtain a precipitate, filter and dry the precipitate to obtain 3-hydroxy-2-nitropyridine.

Embodiment 2

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

[0018] (1) Add concentrated sulfuric acid to 3-hydroxypyridine while stirring, and volatilize hydrogen chloride under reduced pressure, then add oleum and fuming nitric acid with a mass percentage of 45%, heat up to 84°C and stir for 4.5 hours, get the mixture;

[0019] (2) Add concentrated ammonia water dropwise to the mixture, adjust the pH value to make the pH value 5.3, then add water and stir to obtain a precipitate, filter and dry the precipitate to obtain 3-hydroxy-2-nitropyridine.

Embodiment 3

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

[0022] (1) Add concentrated sulfuric acid to 3-hydroxypyridine while stirring, and volatilize hydrogen chloride under reduced pressure, then add 48% by mass of oleum and fuming nitric acid, heat up to 87°C and stir for 3.5 hours, get the mixture;

[0023] (2) Add concentrated ammonia water dropwise to the mixture, adjust the pH value to make the pH value 5, then add water and stir to obtain a precipitate, filter and dry the precipitate to obtain 3-hydroxy-2-nitropyridine.

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PUM

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Abstract

The invention discloses a preparation method of 3-hydroxy-2-nitropyridine. The method comprises the following steps: adding concentrated sulfuric acid into 3-hydroxypyridine while stirring, volatilizing hydrogen chloride under vacuum condition, then adding the fuming sulfuric acid and fuming nitric acid, heating and stirring for 3-5 h to obtain a mixture; dropwise adding concentrated ammonia water into the mixture, adjusting the pH value to 5-5.5, then adding water and stirring to obtain a precipitate, and filtering and drying the precipitate to obtain 3-hydroxy-2-nitropyridine. Through the above way, the preparation method of 3-hydroxy-2-nitropyridine provided by the invention requires short preparation time, saves energy loss in the reaction process, reduces the risk of the synthesis process and greatly reduces the production cost. The obtained 3-hydroxy-2-nitropyridine with high purity can be directly used in a next step.

Description

technical field [0001] The invention relates to the field of fine organic synthesis, in particular to a preparation method of 3-hydroxy-2-nitropyridine. Background technique [0002] Pyridine is a six-membered heterocyclic compound containing a nitrogen atom, that is, one carbon of the benzene molecule is replaced by nitrogen, and it has many special medicinal effects and structural properties. Pyridine derivatives widely exist in nature, many of which have special pharmacological effects. At present, pyridine compounds are mainly obtained by chemical synthesis. The molecular weight of 3-hydroxy-2-nitropyridine is C 5 h 4 N 2 o 3 , with a molecular weight of 140.09 and a melting point of 67-72°C. It is an irritating substance that can irritate the eyes, respiratory system and skin. The reaction time in the traditional synthesis process of 3-hydroxy-2-nitropyridine is long, sometimes even one day, which is prone to danger. Contents of the invention [0003] The techn...

Claims

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Application Information

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IPC IPC(8): C07D213/65
CPCC07D213/65
Inventor 陈雪平
Owner 常熟市联创化学有限公司
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