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Method for preparing 2-aminoisonicotinic acid

A technology of isonicotinic acid and amino group, applied in the field of preparing 2-aminoisonicotinic acid, can solve problems such as the yield of only 5%, and achieve the effects of low price, mild reaction adjustment and good economic benefits

Inactive Publication Date: 2011-11-23
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the synthesis of 2-aminoisonicotinic acid is mainly obtained from 2-amino-4-picoline as raw material through oxidation with potassium permanganate after protecting the amino group, but the yield is only about 5%.

Method used

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  • Method for preparing 2-aminoisonicotinic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0016] (1) Put 5Kg of 2-amino-4-picoline into a 20L spherical reactor, then add 4.2Kg of glacial acetic acid (2-amino-4-picoline is insoluble) and drop 6.65Kg of acetyl chloride into the Reaction system, the reaction produces a large amount of white smoke, the dripping speed should not be too fast. The raw materials will dissolve during the dropwise addition of acetyl chloride, and after the dropwise addition, heat to reflux at 110° C. for 12 hours. After the reaction, stop heating and cool down in the reactor. When a certain amount of crystals are precipitated, put them in water (about 70°C) and continue to cool down to crystallize. Stir frequently during the crystallization process, otherwise they will stick together and suction filtration will be difficult. . After room temperature, filter with suction. The filtrate should be kept, and the unseparated crystals in it can be distilled under reduced pressure after the batch is completed, and the crystals can also be precipit...

Embodiment 2

[0019] (1) Put 5Kg of 2-amino-4-picoline into a 20L spherical reactor, then add 4.6Kg of glacial acetic acid (2-amino-4-picoline is insoluble) and drop 6.3Kg of acetyl chloride into the Reaction system, the reaction produces a large amount of white smoke, the dripping speed should not be too fast. The raw materials will dissolve during the dropwise addition of acetyl chloride, and after the dropwise addition, heat to reflux at 105°C for 13 hours. After the reaction, stop heating and cool down in the reactor. When a certain amount of crystals are precipitated, put them in water (about 70°C) and continue to cool down to crystallize. Stir frequently during the crystallization process, otherwise they will stick together and suction filtration will be difficult. . After room temperature, filter with suction. The filtrate should be kept, and the unseparated crystals in it can be distilled under reduced pressure after the batch is completed, and the crystals can also be precipitate...

Embodiment 3

[0022] (1) Put 5Kg of 2-amino-4-picoline into a 20L spherical reactor, then add 5Kg of glacial acetic acid (2-amino-4-picoline is insoluble) and drop 6.65Kg of acetyl chloride into the reaction while stirring system, the reaction produces a large amount of white smoke, and the dripping speed should not be too fast. The raw materials will dissolve during the dropwise addition of acetyl chloride, and after the dropwise addition, heat to reflux at 110° C. for 12 hours. After the reaction, stop heating and cool down in the reactor. When a certain amount of crystals are precipitated, put them in water (about 70°C) and continue to cool down to crystallize. Stir frequently during the crystallization process, otherwise they will stick together and suction filtration will be difficult. . After room temperature, filter with suction. The filtrate should be kept, and the unseparated crystals in it can be distilled under reduced pressure after the batch is completed, and the crystals can...

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Abstract

The invention discloses a method for preparing 2-aminoisonicotinic acid. 2-amino-4-methylpyridine is used as a raw material. The method comprises the following steps of: protecting amino in acetic acid by acetylation of acetyl chloride, oxidizing methyl in potassium permanganate under the action of a catalyst, performing hydrolysis by using sodium hydroxide, and performing neutralization by using concentrated hydrochloric acid to obtain the 2-aminoisonicotinic acid. The raw materials used in the method are cheap, particularly the yield is improved after the catalyst is added, the utilization rate of raw materials is increased, and the method has good economic benefit.

Description

technical field [0001] The invention relates to a method for preparing 2-aminoisonicotinic acid by using 2-amino-4-picoline as raw material. Background technique [0002] 2-Aminoisonicotinic acid is one of the derivatives of isonicotinic acid. It is an important organic intermediate for medicines and pesticides, especially for the preparation of isoniazid derivatives in medicine. research value. [0003] At present, the synthesis of 2-aminoisonicotinic acid is mainly obtained by using 2-amino-4-picoline as raw material through oxidation with potassium permanganate after protecting the amino group, but the yield is only about 5%. Contents of the invention [0004] The object of the present invention is to provide a kind of use 2-amino-4-picoline as raw material, first protect the amino group with acetyl chloride acetylation in acetic acid, then use potassium permanganate to oxidize the methyl group under the action of a catalyst, and finally use A method for preparing ...

Claims

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Application Information

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IPC IPC(8): C07D213/79C07D213/803
Inventor 邓旭忠黄顺
Owner GUANGDONG UNIV OF TECH
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