Preparation method of 2-chloro-5-chloromethylpyridine

A technology of chloromethylpyridine and dichloromethylpyridine, which is applied in the field of synthesis of 2-chloro-5-chloromethylpyridine, can solve the problems of unsatisfactory yield, difficulty in product separation, and high energy consumption, and achieves satisfactory results. The effect of clean production, high product yield and high content

Inactive Publication Date: 2016-12-21
NANJING REDSUN BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The biggest advantage of the cyclopentadiene route is that it ensures the quality of 2-chloro-5-chloromethylpyridine and greatly reduces its production cost. The disadvantage of this route is that there are too many three wastes, which adds a lot to environmental governance. pressure
Synthesize 2-chloro-5-chloromethylpyridine with 2-chloro-5-methylpyridine. Most of the traditional processes are stirred reactors, which are prepared by adding catalyst azobisisobutyronitrile to catalyze chlorination. The resulting product It is a mixture of 2-chloro-5-methylpyridine, 2-chloro-5-chloromethylpyridine, 2-chloro-5-dichloromethylpyridine, etc., which causes great difficulties in product separation
In addition, the sealing performance of the reaction is poor, the noise is large, the energy consumption is high, the yield is not ideal, and the material is not mixed uniformly.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Add 350g of 2-chloro-5-methylpyridine into a 500ml four-necked flask, stir and heat it under the condition of 80-85°C, feed in chlorine for 8 hours, and analyze 2-chloro-5-dichloromethylpyridine in the central control< 3wt%, cooling down after stopping the reaction, analyzing the content of 2-chloro-5-methylpyridine, 2-chloro-5-chloromethylpyridine and 2-chloro-5-dichloromethylpyridine in the feed liquid, 2- The yield of chloro-5-chloromethylpyridine (calculated as 2-chloro-5-methylpyridine) was 92.3%.

Embodiment 2

[0013] Add 350g of 2-chloro-5-methylpyridine into a 500ml four-necked flask, stir and heat it under the condition of 95-100°C, and react with chlorine gas for 6.5 hours. The central control analysis of 2-chloro-5-dichloromethylpyridine< 3wt%, cooling down after stopping the reaction, analyzing the content of 2-chloro-5-methylpyridine, 2-chloro-5-chloromethylpyridine and 2-chloro-5-dichloromethylpyridine in the feed liquid, 2- The yield of chloro-5-chloromethylpyridine (calculated as 2-chloro-5-methylpyridine) was 92.7%.

Embodiment 3

[0015] Add 350g of 2-chloro-5-methylpyridine into a 500ml four-necked flask, stir and heat it under the condition of 115-120°C, and react with chlorine gas for 5.5 hours. The central control analysis of 2-chloro-5-dichloromethylpyridine< 3wt%, cooling down after stopping the reaction, analyzing the content of 2-chloro-5-methylpyridine, 2-chloro-5-chloromethylpyridine and 2-chloro-5-dichloromethylpyridine in the feed liquid, 2- The yield of chloro-5-chloromethylpyridine (calculated as 2-chloro-5-methylpyridine) was 93.5%.

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PUM

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Abstract

The invention discloses a preparation method of 2-chloro-5-chloromethylpyridine; with 2-chloro-5-methylpyridine as a raw material, the temperature rises to 80-160 DEG C, chlorine gas is introduced, a chlorination reaction is performed, and 2-chloro-5-chloromethylpyridine is obtained. The preparation process adopts heat chlorination, has no need of ultraviolet light catalysis having high energy consumption, also has no need of expensive catalysts, is friendly to the environment and high in product yield, meets the requirements of cleaning production, and is an effective method for preparing 2-chloro-5-chloromethylpyridine.

Description

technical field [0001] The invention relates to a synthesis method of 2-chloro-5-chloromethylpyridine. Background technique [0002] 2-Chloro-5-chloromethylpyridine is a key intermediate for the synthesis of various pesticides, and it is also the most insecticidally active structural part of this class of pesticide molecules. 2-Chloro-5-chloromethylpyridine can not only easily Imidacloprid can be prepared efficiently, and a series of new insecticides and acaricides can also be prepared. Most of these compounds have strong activity. The control of Ye Qiuchan, rice planthopper, aphid, and moth is very effective. The development of 2-chloro-5-chloromethylpyridine has great practical significance for the development and innovation of new, high-efficiency, low-use, and safe new pesticides. [0003] In the early days, there were three main technological routes for large-scale production of 2-chloro-5-chloromethylpyridine in China: 3-picoline route, morpholine route and benzylamin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/61
CPCC07D213/61
Inventor 钟劲松陈新春蒋剑华王福军丁永山
Owner NANJING REDSUN BIOCHEM CO LTD
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