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Process for synthesizing 2-chloro-5-chloromethylpyridine

A technology for chloromethylpyridine and methylpyridine, which is applied in the chlorination field of synthesizing 2-chloro-5-chloromethylpyridine, can solve problems such as pipeline blockage and discharge, complicated experimental or industrial operation, waste pollution and the like

Inactive Publication Date: 2005-06-29
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These side reactions, especially coking, will not only cause a lot of waste and waste pollution of the main raw materials, but also cause pipeline blockage and difficulty in discharging materials, making experiments or industrial operations very complicated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Example 1: 110 grams of 2-chloro-5-picoline (0.862mol) and 174 grams of 1,2-dichlorobenzene were added to a 500ml chlorination reactor, the temperature was raised to 130°C, and chlorine gas was introduced; Add the initiator azobisisobutyronitrile once every hour, add 0.3 g each time, add altogether 4 times; react at this temperature for 4 hours. After the reaction, turn off the chlorine gas, lower the temperature, switch to nitrogen replacement for 0.5 hours, add sodium hydroxide to neutralize until the pH value is 9-10, separate the water phase, and separate the solvent 1,2-dichlorobenzene by distillation under reduced pressure. The amount of CCMP obtained by rectification of the still liquid was 0.405 mol, the conversion rate of CMP was 56.1%, and the yield of CCMP (based on converted CMP) was 83.9%.

Embodiment 2

[0013] Example 2: 110 grams of 2-chloro-5-picoline (0.862mol) and 174 grams of 1,2-dichlorobenzene were added to a 500ml chlorination reactor, the temperature was raised to 100°C, and chlorine gas was introduced; Add the initiator azobisisobutyronitrile once every hour, add 0.6 gram each time, add altogether 4 times; React at this temperature for 4 hours. The aftertreatment was the same as in Example 1 to obtain a CCMP amount of 0.301 mol, a CMP conversion rate of 39.0%, and a CCMP yield (based on converted CMP) of 89.5%.

Embodiment 3

[0014] Example 3: 110 grams of 2-chloro-5-picoline (0.862mol) and 174 grams of 1,2-dichlorobenzene were added to a 500ml chlorination reactor, the temperature was raised to 150°C, and chlorine gas was introduced; Add the initiator azobisisobutyronitrile once every hour, add 0.6 gram each time, add altogether 4 times; React at this temperature for 4 hours. The aftertreatment was the same as in Example 1 to obtain a CCMP amount of 0.419 mol, a CMP conversion rate of 65.0%, and a CCMP yield (based on converted CMP) of 74.8%.

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Abstract

A method for synthesizing 2-chlorine-5-chloromethyl pyridine, uses 2-chlorine-5- as the raw material, organic chloride as solvent, in the conditions of temperature:80-180deg.C and normal pressure, initiate by chloride or light, through choosing chlorination reaction to synthesize 2-chlorine -5-chloromethyl pyridine directly. The invention has high conversion rate and utilization ratio of raw material little coking in chlorination reaction, and high seletivity and productivity.

Description

technical field [0001] The present invention relates to the preparation of halogen-containing and heterocyclic organic intermediates, and particularly provides a method for synthesizing 2-chloro-5-chloromethylpyridine (abbreviated as CCMP) with 2-chloro-5-methylpyridine (referred to as CMP) as raw material Chlorination method. Background technique [0002] 2-Chloro-5-chloromethylpyridine is an important chlorine-containing and heterocyclic organic intermediate, which has a wide range of uses in fine chemical fields such as pesticides and medicines. The traditional synthesis process is obtained by chlorination of 2-chloro-5-picoline; however, due to the difficulty in controlling the selectivity, the conversion rate and effective utilization of raw materials are low, the chlorination selectivity is not high, and the actual operation is difficult . [0003] USP 5,198,549 introduces a method for the selective chlorination of 2-chloro-5-methylpyridine to synthesize 2-chloro-5-c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/61
Inventor 张伟徐杰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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