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Method for synthesizing 6-chloropyridine-3-carbonyl chloride

A technology of carbonyl chloride and chloropyridine, which is applied in the field of synthesis of 6-chloropyridine-3-carbonyl chloride, can solve the problem of high price of 6-chloropyridine-3-carbonyl chloride, and achieve easy control of industrial production, mild reaction conditions, low cost effect

Active Publication Date: 2010-06-09
NANJING REDSUN BIOCHEM CO LTD +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] 6-chloropyridine-3-carbonyl chloride is an important chemical and pharmaceutical intermediate, generally obtained from 6-chloropyridine-3-carboxylic acid through acid chlorination, because the price of 6-chloropyridine-3-carboxylic acid itself is relatively high , so the current price of 6-chloropyridine-3-carbonyl chloride is relatively high
At present, there are many reports on the acylchlorination of trichloromethyl groups with ferric chloride and zinc chloride, which are realized on the benzene ring. This method is also relatively mature, and there are no reports on the pyridine ring.

Method used

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  • Method for synthesizing 6-chloropyridine-3-carbonyl chloride
  • Method for synthesizing 6-chloropyridine-3-carbonyl chloride
  • Method for synthesizing 6-chloropyridine-3-carbonyl chloride

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Add 231g of 2-chloro-5-trichloromethylpyridine in a 500ml four-necked reaction flask equipped with an agitator and a thermometer tail gas absorption device, add 11.55g (5%) of ferric chloride, slowly heat up to 95°C, and slowly drop Add 18g of distilled water, after completion of the dropwise addition, heat-preserved and stirred for 8 hours, after the reaction, the reaction solution was directly distilled under reduced pressure, collected at 83-85°C / 3mmHg, and 170.2g of a solid with a white melting point of 50°C was obtained, of which 6 -Chloropyridine-3-carbonyl chloride has a purity of 97.4% and an actual yield of 94.1%.

Embodiment 2～4

[0021] Reaction technology is identical with example 1, and the molar ratio of water and 2-chloro-5-trichloromethylpyridine is 1: 1, and concrete process parameter and result are shown in Table 1:

[0022] Process parameter and result of table 1 embodiment 2~4

[0023]

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PUM

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Abstract

The invention discloses a method for synthesizing 6-chloropyridine-3-carbonyl chloride, and 2-chloro-5-trichloromethylpyridine is mixed with a solvent and a catalyst for hydrolysis reaction under the temperature of 60-150 DEG C, thus preparing the 6-chloropyridine-3-carbonyl chloride. 6-chloropyridine-3-carboxylic acid with an expensive price is avoided to being used in the synthesis of the 6-chloropyridine-3-carbonyl chloride, instead, 2-chloro-5-(trifluoromethyl)pyridine with a low price is used, and the synthesis method in the invention has the characteristics of mild reaction conditions, simple technology, high yield, easily-controlled industrial production, low cost of the catalyst and low pollution.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and in particular relates to a synthesis method of 6-chloropyridine-3-carbonyl chloride. Background technique [0002] 6-chloropyridine-3-carbonyl chloride is an important chemical and pharmaceutical intermediate, which is generally obtained from 6-chloropyridine-3-carboxylic acid through acid chlorination, because the price of 6-chloropyridine-3-carboxylic acid itself is relatively high , so the current price of 6-chloropyridine-3-carbonyl chloride is relatively high. [0003] 2-Chloro-5-trichloromethylpyridine is generally used in the synthesis of pesticides because it has many industrial applications and its production technology is relatively mature. At present, there are many reports on the acylchlorination of trichloromethyl groups with ferric chloride and zinc chloride, which are realized on the benzene ring. This method is relatively mature, and there is no report on the pyr...

Claims

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Application Information

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IPC IPC(8): C07D213/80C07D213/803
Inventor 王述刚杜翔张阿金俞建良陈金福
Owner NANJING REDSUN BIOCHEM CO LTD
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