A method for synthesizing 2,6-pyridinedicarboxylic acid

A technology of dipicolinic acid and dichloropyridine, which is applied in the development of pharmaceutical intermediates and the field of pesticides, can solve the problems of high cost and high price, and achieve the effect of low environmental pollution, great cost advantage and environmental friendliness

Inactive Publication Date: 2019-08-16
NANJING REDSUN BIOCHEM CO LTD
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  • Abstract
  • Description
  • 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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  • A method for synthesizing 2,6-pyridinedicarboxylic acid
  • A method for synthesizing 2,6-pyridinedicarboxylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Dissolve 148g (1mol) of 2,6-dichloropyridine in 721g (10mol) of tetrahydrofuran solution, add 60g (2.5mol) of magnesium powder, pass through nitrogen to isolate the air, and heat the solution to 55°C while stirring (ie 2, The reaction temperature of 6-dichloropyridine and active metal is 55°C), add 0.55g (0.005mol) of initiator dibromoethane, stir and react 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; cool down to -15°C, slowly pass in excess dry carbon dioxide gas, judge the reaction according to the flow rate of carbon dioxide, judge the end of the reaction when the amount of carbon dioxide entering is the same as that of the tail gas, and acidify the solution after the end , filtered to remove tetrahydrofuran to obtain 2,6-pyridinedicarboxylic acid with a yield of 94.5% and a purity of 97% after extraction,

Embodiment 2

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

Embodiment 3

[0025] Except that before adding the initiator, the solution was heated to 60°C (that is, the temperature for the interaction between 2,6-dichloropyridine and the active metal was 60°C), the rest of the reaction conditions were 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, in particular to a method for synthesizing 2,6-pyridinedicarboxylic acid. Background technique [0002] 2,6-pyridinedicarboxylic acid is an important pesticide and pharmaceutical intermediate, which exists in large quantities in bacterial spores. At present, 2,6-pyridinedicarboxylic acid is mainly obtained through biological extraction or 2,6-bis Oxidation of the methyl group is obtained. Regardless of the method, the cost is relatively high, resulting in the high price of 2,6-pyridinedicarboxylic acid in the current market. [0003] Due to the increase in domestic pyridine production capacity and the increased demand for chloropyridine, a large amount of pyridine is chlorinated to obtain different chlorinated products, and 2,6 dichloropyridine appears as a by-product of pyridine chlorinated products in large quantities, with a relatively low The price a...

Claims

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Application Information

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Patent Type & Authority Patents(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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