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Synthesis method of 2-chloro-5-chloromethyl pyridine

A technology of chloromethylpyridine and methylpyridine is applied in the field of synthesis of 2-chloro-5-chloromethylpyridine, and can solve the problems of poor sealing performance, high noise, unsatisfactory yield and the like

Inactive Publication Date: 2004-08-04
TIANJIN UNIV
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  • Abstract
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Problems solved by technology

[0003] Known synthetic method of producing 2-chloro-5-chloromethylpyridine, it takes 2-chloro-5-methylpyridine as raw material, through catalytic chlorination, directly synthesizes 2-chloro-5-chloromethylpyridine, traditional Most of the reactors used in the process are stirred tank reactors, which have poor sealing performance, high noise, high energy consumption, unsatisfactory yield, and difficult material mixing.

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  • Synthesis method of 2-chloro-5-chloromethyl pyridine
  • Synthesis method of 2-chloro-5-chloromethyl pyridine

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Embodiment Construction

[0013] The present invention will be further described below in conjunction with embodiment:

[0014] 1. Add 2-chloro-5-picoline and carbon tetrachloride solvent in the air-lift loop reactor so that the concentration of 2-chloro-5-picoline is 0.33g / ml; the pressure is 745~750mmHg Under certain conditions, dry nitrogen is sprayed into the airlift loop reactor from the bottom of the airlift loop reactor to form an internal circulation flow, and the reactant and solvent are mixed evenly; the catalyst azobisisobutyronitrile is added to make The molar ratio of it to 2-chloro-5-picoline is 1:20, the temperature is raised to 75°C, the solvent is in a reflux state, and nitrogen gas is continued at this temperature for 5 minutes; nitrogen gas flow is stopped, and dry Chlorine gas, make chlorine gas form a liquid internal circulation flow in the air-lift loop reactor, the speed of chlorine gas flow is 300 ~ 400ml / min, and online detection of 2-chloro-5-picoline and 2-chloro-5 - the pur...

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Abstract

A process for synthesizing 2-chloro-5-chloromethyl pyridine includes such steps as adding 2-chloro-5-methyl pyridine and CC4 solvent into airlift recirculating reactor, spraying dry N2 into the reactor from its bottom under micro negative pressure, adding azadiisobutylnitrie as catalyst, heating to 70-80 deg.C, continuously introducing N2 for 2-10 min, stopping the introduction of N2, and introducing dry chlorine gas and in-line detection with gas-phase chromatograph. Its advantages are less consumption of chlorine gas and short time of supplying chlorine gas.

Description

technical field [0001] The invention relates to a synthesis method of 2-chloro-5-chloromethylpyridine. technical background [0002] Currently, 3-methylpyridine insecticides represented by imidacloprid, acetamiprid, fluazifop-p-butyl, and valalifop, have systemic , broad spectrum, high efficiency, long duration, good safety and other advantages, has been widely used at home and abroad, and 2-chloro-5 chloromethylpyridine is the key intermediate for the synthesis of the above pesticides. [0003] Known synthetic method of producing 2-chloro-5-chloromethylpyridine, it takes 2-chloro-5-methylpyridine as raw material, through catalytic chlorination, directly synthesizes 2-chloro-5-chloromethylpyridine, traditional Most of the reactors used in the process are stirred tank reactors, which have poor sealing performance, high noise, high energy consumption, unsatisfactory yield, and difficult uniform mixing of materials. ...

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Application Information

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IPC IPC(8): C07D213/61
Inventor 闻建平毛国柱乔萍韩巍潘磊王长林
Owner TIANJIN UNIV
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