Method for electrolytic synthesis of 4-amino-3,6-dichloropyridine-2-carboxylic acid

A technology of dichloropyridine and electrolytic synthesis, which is applied in the direction of electrolytic process, electrolytic components, electrolytic organic production, etc., can solve the problems of difficult control of the reaction, expensive raw materials used, unfriendly environment, etc., and achieve less investment and reduced side effects of industrial production. Reaction, the effect of no three wastes pollution

A technology of dichloropyridine and electrolytic synthesis, which is applied in the direction of electrolytic process, electrolytic components, electrolytic organic production, etc., can solve the problems of difficult control of the reaction, expensive raw materials used, unfriendly environment, etc., and achieve less investment and reduced side effects of industrial production. Reaction, the effect of no three wastes pollution

CN101575712AInactive Publication Date: 2009-11-11HUNAN XIANGDA BIDE CHEM
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  • Method for electrolytic synthesis of 4-amino-3,6-dichloropyridine-2-carboxylic acid
  • Method for electrolytic synthesis of 4-amino-3,6-dichloropyridine-2-carboxylic acid
  • Method for electrolytic synthesis of 4-amino-3,6-dichloropyridine-2-carboxylic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Prepare 450ml electrolyte solution, which contains 95.5% 4-amino-3,5,6-trichloropyridine-2-carboxylic acid 33g, containing 1.5% sodium hydroxide, and the electrolyte solution is under magnetic stirring, and the constant potential electrolysis power supply is turned on, and the control The potential of the saturated calomel reference electrode is between -1100mv~-1350mv, after adding 32% sodium hydroxide solution for 24 hours, sampling and analysis, when the content of 4-amino-3,5,6-trichloropyridine-2-carboxylic acid When it is less than 0.6%, stop the power supply and stop the reaction; the electrolyte is neutralized with 36% hydrochloric acid, concentrated in vacuum below 65°C to 180ml, cooled to normal temperature, filtered, washed 3 times with 20ml water (total water volume 60ml), 80°C After drying, 23.17 g of the product was obtained. Through high-performance liquid chromatography analysis, the content was 94%, the melting point was 185-189° C., and the yield was 81...

Embodiment 2

[0035] According to embodiment 1, replace sodium hydroxide with potassium hydroxide, alkalinity is controlled at 1.0%~1.5%, and reaction temperature is controlled at 20 ℃, and the total consuming time of reaction completion is 22 hours, and aftertreatment method is the same as above, obtains product 25.1g, The content is 96.5%, the melting point is 184-187°C, and the yield is 90%.

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Abstract

The invention discloses a method for electrolytic synthesis of 4-amino-3,6-dichloropyridine-2-carboxylic acid, which comprises: taking 4-amino-3,5,6-trichloropyridine-2-carboxylic acid (picloram) as a raw material, and performing selective dechlorination on the raw material through electrolysis; and acidifying, filtering and drying electrolyte after the electrolytic reaction is over, and obtaining the target compound, namely the 4-amino-3,6-dichloropyridine-2-carboxylic acid, wherein the electrolytic reaction is performed at normal temperature, and the alkalinity of the electrolyte is between 0.5 and 2.0 percent. The method has good reaction selectivity, high purity of the synthesized target compound, and simple process, has the reaction performed at normal temperature and normal pressure, effectively reduces the occurrence of side reactions of hydroxylation and amino oxidation, has less investment when being used for industrial production, and basically has no pollution of the three wastes.

Description

technical field [0001] The invention belongs to the field of organic electrochemical synthesis and relates to an electrolytic synthesis method of 4-amino-3,6-dichloropyridine-2-carboxylic acid. Background technique [0002] 4-Amino-3,6-dichloropyridine-2-carboxylic acid, trade name Aminazopyr, Aminopyralid, Dichloroaminopyridine, is a pyridinecarboxylic acid herbicide, it can quickly enter the plant In vivo, it is easily absorbed by stems and leaves, resulting in growth interruption and rapid necrosis. It is mainly used for weed control in pastures, plantations and non-crop areas, and for weeding in rapeseed and buckwheat fields. [0003] The electrolytic reduction method is currently the most effective synthesis method for 4-amino-3,6-dichloropyridine-2-carboxylic acid. US Patent USP6352635 discloses the use of electrolytic reduction method to synthesize 4-aminopyridine acid. This patent also involves 4-aminopyridine - The electrolytic synthesis method of 3,6-dichloropyri...

Claims

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Application Information

Patent Timeline
11 Nov 2009
Publication
CN101575712A
IPC
C25B3/04; C25B3/25
Inventors
王良芥; 朱昭健