Method for synthesizing 2,6-dipicolinic acid

A technology of dipicolinic acid and dichloropyridine, which is applied in the development of pharmaceutical intermediates and pesticide fields, can solve the problems of high price and high cost, and achieve the effects of large cost advantage, low environmental pollution and environmental friendliness.

Inactive Publication Date: 2016-12-07
NANJING REDSUN BIOCHEM CO LTD
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

Regardless of the method, its cost is high, resulting in the high price of 2,6-pyridinedicarboxylic acid in the current market

Method used

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  • Method for synthesizing 2,6-dipicolinic acid
  • Method for synthesizing 2,6-dipicolinic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 148g (1mol) 2,6-dichloropyridine was dissolved in 721g (10mol) tetrahydrofuran solution, 60g (2.5mol) magnesium powder was added, nitrogen was introduced to isolate the air, and the solution was heated while stirring to 55°C (ie 2, The reaction temperature of 6-dichloropyridine and active metal is 55℃), 0.55g (0.005mol) of initiator dibromoethane is added, and the reaction is carried out with stirring for 6 hours (that is, the reaction time of 2,6-dichloropyridine and active metal is 6 hours), the solution after the reaction is transparent; the temperature is lowered to -15°C, and excessive dry carbon dioxide gas is slowly introduced. The reaction is judged according to the carbon dioxide flow rate. When the amount of carbon dioxide and the exhaust gas are the same, the reaction is judged to be over, and the solution is acidified after the end , Filter and remove tetrahydrofuran to obtain 2,6-pyridinedicarboxylic acid with a yield of 94.5% and a purity of 97% after extrac...

Embodiment 2

[0023] Except that before adding the initiator, the solution was heated to 30°C (that is, the temperature of 2,6-dichloropyridine and the active metal is 30°C), and the rest of the reaction conditions are exactly the same as in Example 1. After the reaction, 2, The yield of 6-pyridinedicarboxylic acid was 92%, and the purity after extraction was 75.2%.

Embodiment 3

[0025] Except that before adding the initiator, the solution was heated to 60°C (that is, the temperature of 2,6-dichloropyridine and the active metal is 60°C), the rest of the reaction conditions are exactly the same as in Example 1. After the reaction, 2 ,6-pyridinedicarboxylic acid, the yield was 93.8%, and the purity after extraction was 94.3%.

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Abstract

The invention discloses a method for synthesizing 2,6-dipicolinic acid. The method comprises the following steps: under the condition of air isolation, by using anhydrous diethyl ether or THF (tetrahydrofuran) as solvent, reacting 2,6-dichloropyridine used as a raw material with active metal under the action of an initiator to obtain a Grignard reagent; and cooling, then introducing excessive dry carbon dioxide gas, and acidifying to obtain the 2,6-dipicolinic acid. According to the invention, the cheap 2,6-dichloropyridine is used as the raw material, so the cost is low; and the synthesis process route is simple and easy to control, and can easily implement industrial production.

Description

Technical field [0001] The invention belongs to the field of development of pesticides and pharmaceutical intermediates, and particularly relates to a method for synthesizing 2,6-pyridinedicarboxylic acid. Background technique [0002] 2,6-Dipicolinic acid is an important pesticide and pharmaceutical intermediate. It exists in large quantities in the spores of bacteria. At present, 2,6-dipicolinic acid is mainly obtained through biological extraction or 2,6-dipicolinic acid. Methyl oxidation is obtained. Regardless of the method, the cost is relatively high, leading to the high price of 2,6-pyridinedicarboxylic acid in the current market. [0003] Due to the increase in domestic pyridine production capacity and the increasing demand for chloropyridine, a large amount of pyridine is chlorinated to obtain different chlorinated products, and 2,6 dichloropyridine has become a large number of by-products of pyridine chlorination products. The price advantage has become a cheap raw mat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/79C07D213/803
CPCC07D213/79C07D213/803
Inventor 王述刚江涛蒋剑华陈新春
Owner NANJING REDSUN BIOCHEM CO LTD
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