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Synthesis method of 4-amino-3,6-dichloropyridine-2-formic acid

A technology of dichloropyridine and synthesis method, applied in diaphragm, electrolysis process, organic chemistry, etc., can solve problems affecting product quality, etc., and achieve the effects of prolonging electrode life, reducing impurities, and reducing cleaning frequency

Active Publication Date: 2018-10-02
LIER CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, in the actual production process, the applicant found that the appearance of 4-amino-3,6-dichloropyridine-2-carboxylic acid obtained by electrolysis, acidification and crystallization was brownish red, which seriously affected the product quality

Method used

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  • Synthesis method of 4-amino-3,6-dichloropyridine-2-formic acid
  • Synthesis method of 4-amino-3,6-dichloropyridine-2-formic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0032] In this example, the type of cationic membrane is Air-Environment-IONSEP-Dry (cation membrane, red). Add 240mL3.0wt% sodium hydroxide solution in the anode area of ​​the reactor, and add 240mL7wt% 4-amino-3,5,6-trichloropyridine-2-sodium formate aqueous solution (containing 4-amino-3,5, 6-trichloropyridine-2-carboxylic acid 0.075mol).

[0033] The electrolytic reaction is carried out at a temperature of 10-50° C. and a potential difference between the cathode plate and its surface of -1.00--1.40 V through a direct current power supply. During the reaction process, 3 g of solid sodium hydroxide (containing 0.075 mol of sodium hydroxide) was gradually added to the anode area. The electrolysis reaction continues until the conversion rate of raw materials reaches the specified value, and then the electrolysis is stopped.

[0034] The reaction solution in the cathode area was filtered and then transferred to the acidification tank, and the pH value of the system was adjust...

Embodiment 2

[0036] In this example, the type of cationic membrane is Air-Environment-IONSEP-Dry (cationic membrane, yellow). Add 240mL3.0wt% sodium hydroxide solution in the anode area of ​​the reactor, and add 240mL10wt% 4-amino-3,5,6-trichloropyridine-2-sodium formate aqueous solution (containing 4-amino-3,5, 6-trichloropyridine-2-carboxylic acid 0.1 mol).

[0037] The electrolytic reaction is carried out at a temperature of 10-50° C. and a potential difference between the cathode plate and its surface of -1.00--1.40 V through a direct current power supply. During the reaction process, 4 g of solid sodium hydroxide (containing 0.1 mol of sodium hydroxide) was gradually added to the anode area. The electrolysis reaction continues until the conversion rate of raw materials reaches the specified value, and then the electrolysis is stopped.

[0038] After filtering the reaction solution in the cathode area, it was transferred to an acidification tank, and the pH value of the system was ad...

Embodiment approach

[0041] The specific implementation method is as follows. Add 240mL6.0wt% sodium hydroxide solution, 240mL7wt% 4-amino-3,5,6-trichloropyridine-2-sodium formate aqueous solution (containing 4-amino-3,5,6-trichloro pyridine-2-carboxylic acid 0.075 mol).

[0042] The electrolytic reaction is carried out at a temperature of 10-50° C. and a potential difference between the cathode plate and its surface of -1.00--1.40 V through a direct current power supply. During the reaction process, 3 g of solid sodium hydroxide (containing 0.075 mol of sodium hydroxide) was gradually added to the anode area. The electrolysis reaction continues until the conversion rate of raw materials reaches the specified value, and then the electrolysis is stopped.

[0043] The reaction solution in the cathode area was filtered and transferred to the acidification tank, and the pH value of the system was adjusted to 1.0 with hydrochloric acid. After filtering, it was dried to obtain 14.4 g of brown-red amin...

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Abstract

The invention discloses a synthesis method of 4-amino-3,6-dichloropyridine-2-formic acid and aims to solve the problem that when the 4-amino-3,6-dichloropyridine-2-formic acid is prepared through electrolysis, acidification and crystallization at present, a product has brownish red appearance and the quality of the product is severely affected. By adopting some special cation membranes to divide an electrolytic tank into independent anode and cathode areas, the effect of electrolytic dechloridation is not affected, it can be also avoided that oxidation reaction occurs on anode surfaces to generate oxygen (or high-activity free radicals), the oxygen is in contact with 4-amino-3,6-dichloropyridine-2-formate and accordingly no brownish red impurity is generated. Processes of posttreatment aregreatly simplified, and the costs of posttreatment are decreased.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for synthesizing 4-amino-3,6-dichloropyridine-2-carboxylic acid. Background technique [0002] The use of 4-amino-3,6-dichloropyridine-2-carboxylic acid as a herbicide has been disclosed by patent WO01 / 51468. The synthesis method of the compound has been disclosed by patents CN102597328, CN101522628 and CN1394241. At present, the existing 4-amino-3,6-dichloropyridine-2-carboxylic acid is obtained from 4-amino-3,5,6-trichloropyridine-2-carboxylic acid through electrolytic dechlorination. [0003] However, in the actual production process, the applicant found that the appearance of 4-amino-3,6-dichloropyridine-2-carboxylic acid obtained through electrolysis, acidification and crystallization was brownish red, which seriously affected the product quality. [0004] Therefore, a new method is urgently needed to solve the above problems. Contents of the invention [0005]...

Claims

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Application Information

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IPC IPC(8): C25B3/00C25B13/02C07D213/79
CPCC07D213/79C25B3/00C25B13/02
Inventor 任杰李建伟刘强
Owner LIER CHEM CO LTD
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