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Synthesis method of 2-picolinic acid

A technology of picolinic acid and synthesis method, applied in the direction of organic chemistry and the like, can solve problems such as strong corrosion of equipment, low purity, difficult handling, etc., and achieve the effects of easy operation, high product yield and simple process

Inactive Publication Date: 2009-12-16
NANTONG ACETIC ACID CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 3. 2-pyridinecarboxylic acid can also be obtained by sulfuric acid oxidation using 2-picoline as raw material, but this process will produce a large amount of waste acid, which is difficult to handle
[0006] The purification process includes benzene method, water phase method, acetic acid method and ethanol method. The amount of solvent consumed by the benzene method is too large, about 10 times that of the ethanol method, and the purity of the product of the water phase method is not high. Although the product quality of the acetic acid method is good, However, acetic acid is a strong acid, which is extremely corrosive to equipment and is not conducive to safe production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] In a 500ml three-necked flask, add 100g of 2-cyanopyridine and 200g of deionized water, then start stirring, heat up to 50°C, add 128.2g of 30% sodium hydroxide to the flask, after the addition is complete, then Continue to heat up, reflux reaction for 4 hours, then distill water, after distilling 50g of water, cool the reaction solution to 20°C, add 30% hydrochloric acid, adjust the pH value of the reaction solution at 2.5, then turn on the steam to raise the temperature and distill water, and steam to the kettle When the temperature reaches 120°C, the reaction solution is evaporated to dryness, and the steaming is completed, and then 300g of absolute alcohol is added dropwise to the flask to maintain the temperature of the reaction solution at 55°C. After the addition is completed, stir and dissolve for 2 hours, then filter, and the filtrate After cooling and crystallization, solid 2-picolinic acid was precipitated, filtered and dried to obtain 106.0 g of 2-picolinic a...

Embodiment 2

[0016] On the basis of Example 1, the 30% sodium hydroxide used for the reaction was increased to 141.0g, and the reflux reaction time was increased to 6 hours, and other conditions were the same as in Example 1 to obtain 108.1g of 2-pyridinecarboxylic acid, and the yield was 91.4%.

Embodiment 3

[0018] On the basis of Example 1, the 30% sodium hydroxide used for the reaction was increased to 153.8g, the reflux reaction time was increased to 10 hours, the amount of distilled water was 100g, the pH value was adjusted to 3.5 by adding 30% hydrochloric acid, and the evaporation temperature was The temperature was increased to 130° C., and other conditions were the same as in Example 1 to obtain 107.2 g of 2-pyridinecarboxylic acid with a yield of 90.6%.

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PUM

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Abstract

The invention discloses a synthesis method of 2-picolinic acid, which is implemented by hydrolyzing 2-cyanopyridine under alkaline condition, then using acid to neutralize, and steaming for drying followed by extracting with ethanol to obtain 2-picolinic acid. The invention is simple in technique, easy in operation and high in product yield.

Description

Technical field: [0001] The invention relates to a method for synthesizing 2-pyridinecarboxylic acid. Background technique: [0002] Existing methods for preparing 2-picolinic acid include: [0003] 1. Using 2-picoline as a raw material to oxidize potassium permanganate to obtain 2-pyridinecarboxylic acid, and then extract it with a solvent. According to literature reports, the final yield is only less than 70%. [0004] 2. Using 2-vinylpyridine as a raw material, potassium permanganate is oxidized to obtain 2-pyridinecarboxylic acid, and then extracted. Since there are many side reactions in this reaction, several recrystallizations are required to obtain a qualified product. [0005] 3. 2-pyridinecarboxylic acid can also be obtained by sulfuric acid oxidation with 2-picoline as raw material, but this process will produce a large amount of waste acid, which is difficult to handle. [0006] The purification process includes benzene method, water phase method, acetic acid m...

Claims

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Application Information

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IPC IPC(8): C07D213/803C07D213/79
Inventor 丁彩峰朱小刚刘芳周新建薛建锋
Owner NANTONG ACETIC ACID CHEM
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