Novel method for synthesizing 2-chloronicotinic acid

A synthetic method, the technology of chloronicotinic acid, applied in the direction of organic chemistry, etc., can solve the problems of low yield and large amount of acid used, and achieve the effect of high yield, simple process and clean production

Active Publication Date: 2011-04-06
JIANGSU ZHONGBANG PHARMA
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

But hydrolyzing 2-chloro-3-trichloromethylpyridine in concentrated acid to prepare 2-chloronicotinic acid, the yield is relatively low, and the usage of acid is very large

Method used

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  • Novel method for synthesizing 2-chloronicotinic acid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 10.0g (0.0433mol) of 2-chloro-3-trichloromethylpyridine, 100g of water, and 7.5g (0.1875mol) of sodium hydroxide were added to a 250ml four-neck flask, stirred and heated at 95°C for 4 hours, then stopped After the reaction, cool to room temperature, add concentrated hydrochloric acid to adjust the pH to below 1, there is a large amount of white precipitate, filter with suction, wash, and dry to obtain 6.46g of solid, 2-chloronicotinic acid with a purity of 97.9% and a yield of 92.8%.

Embodiment 2

[0024] 10.0g (0.0433mol) of 2-chloro-3-trichloromethylpyridine, 150g of water, 6.0g (0.15mol) of sodium hydroxide were added to a 250ml four-neck flask, stirred and heated at 50°C for 9 hours, then stopped After the reaction, cool to room temperature, add concentrated hydrochloric acid to adjust the pH to below 1, there is a large amount of white precipitate, filter, wash, and dry to obtain 6.42g of solid, 2-chloronicotinic acid with a purity of 95.2% and a yield of 89.6%.

Embodiment 3

[0026] 10.0g (0.0433mol) of 2-chloro-3-trichloromethylpyridine, 200g of water, and 8.5g (0.0802mol) of sodium carbonate were added to a 250ml four-neck flask, stirred and heated at 85°C for 6 hours, and the reaction was stopped After cooling to room temperature, concentrated hydrochloric acid was added to adjust the pH to below 1. There was a large amount of white precipitate, which was suction filtered, washed, and dried to obtain 6.50 g of solid. The purity of 2-chloronicotinic acid was 96.7%, and the yield was 92.2%.

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Abstract

The invention relates to a novel method for synthesizing 2-chloronicotinic acid. The method comprises the following steps of: taking 2-chloro-3-trichloromethylpyridine as a raw material, decomposing the 2-chloro-3-trichloromethylpyridine in alkaline water solution by heating, cooling down the alkaline water solution and adjusting the solution to acid to obtain a precipitate of the 2-chloronicotinic acid, suction-filtering, washing and drying the precipitate to obtain a white solid powder of the 2-chloronicotinic acid. The method has the advantages of simple and convenient production process and high yield, and the yield is 93 percent by taking the 2-chloro-3-trichloromethylpyridine as a basis.

Description

technical field [0001] The present invention belongs to the technical field of organic chemistry and relates to a new method for synthesizing 2-chloronicotinic acid. Background technique [0002] As an important agricultural and pharmaceutical intermediate, 2-chloronicotinic acid can be used to prepare the new high-efficiency herbicide nicosulfuron, non-steroidal anti-inflammatory drugs, high-efficiency anti-inflammatory analgesics niflufenamic acid, pranosulfur and HIV reverse transcriptase inhibitor nevira etc. These products are in short supply at home and abroad. Therefore, the research on the preparation of 2-chloronicotinic acid is of great significance. [0003] 2-Chloro-5-picoline is the raw material for the synthesis of the pesticide imidacloprid. In the process of synthesizing 2-chloro-5-picoline with 3-picoline as raw material, there is the isomer 2-chloro-3-methyl Pyridine, using the by-product 2-chloro-3-picoline of imidacloprid as raw material to prepare 2-ch...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/80C07D213/803
Inventor 杨寿海钟劲松芮忠南刘善和葛九敢
Owner JIANGSU ZHONGBANG PHARMA
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