Preparation method of 2-fluorine-3-chlorine-5-trifluoromethylpyridine

A technology of trifluoromethylpyridine and trichloromethylpyridine, which is applied in the field of preparation of 2-fluoro-3-chloro-5-trifluoromethylpyridine, can solve the problem of difficulty in separating isomers, difficulty in industrialized production, and side effects. There are many problems such as many products, so as to achieve the effect of simple operation, favorable for large-scale production and low production cost

Inactive Publication Date: 2018-04-20
SHANDONG HUIMENG BIO TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] ②Preparation from 2-amino-5-methylpyridine by bromination and then chlorination. This route is simple in process, but it is difficult to separate isomers;
[0018] T

Method used

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  • Preparation method of 2-fluorine-3-chlorine-5-trifluoromethylpyridine

Examples

Experimental program
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Effect test

Embodiment 1

[0041] Put 2000kg of 2-chloro-5-trichloromethylpyridine into the glass-lined chlorination kettle, then add the catalyst into the reaction kettle and heat the 150kg reaction kettle with heat-conducting oil. When the temperature rises to 130°C, feed chlorine gas into the reaction kettle , Control the amount of chlorine, so that the reaction temperature is controlled at 180 ° C. The reaction time is generally 100 hours. After the reaction is completed, the temperature is lowered to 50°C, the catalyst is filtered out, and 2,3-dichloro-5-trichloromethylpyridine is metered into the fluorination tank for fluorination.

[0042] Put the chlorinated 2,3-dichloro-5-trichloromethylpyridine into the fluorination kettle (about 2300kg), put the catalyst antimony pentafluoride 200kg into the reaction fluorine, add 1700kg of anhydrous hydrogen fluoride, press 2,3 - The molar ratio of dichloro-5-trichloromethylpyridine to hydrogen fluoride is 1:10, and excess hydrogen fluoride is beneficial to ...

Embodiment 2

[0047] Put 2000kg of 2-chloro-5-trichloromethylpyridine into the glass-lined chlorination kettle, then add the catalyst into the reaction kettle and heat the 150kg reaction kettle with heat-conducting oil. When the temperature rises to 130°C, feed chlorine gas into the reaction kettle , Control the amount of chlorine, so that the reaction temperature is controlled at about 190 ° C. The reaction time is generally 70 hours. After the reaction is completed, the temperature is lowered to 50°C, the catalyst is filtered out, and 2,3-dichloro-5-trichloromethylpyridine is metered into the fluorination tank for fluorination.

[0048]Put the chlorinated 2,3-dichloro-5-trichloromethylpyridine into the fluorination kettle (about 2300kg), put the catalyst antimony pentafluoride 200kg into the reaction fluorine, add 1700kg of anhydrous hydrogen fluoride, press 2,3 - The molar ratio of dichloro-5-trichloromethylpyridine to hydrogen fluoride is 1:12, and excess hydrogen fluoride is beneficial...

Embodiment 3

[0051] Put 2000kg of 2-chloro-5-trichloromethylpyridine into the glass-lined chlorination kettle, then add the catalyst into the reaction kettle and heat the 150kg reaction kettle with heat-conducting oil. When the temperature rises to 130°C, feed chlorine gas into the reaction kettle , Control the amount of chlorine, so that the reaction temperature is controlled at about 185 ° C. The reaction time is generally 85 hours. After the reaction is completed, the temperature is lowered to 50°C, the catalyst is filtered out, and 2,3-dichloro-5-trichloromethylpyridine is metered into the fluorination tank for fluorination.

[0052] Put the chlorinated 2,3-dichloro-5-trichloromethylpyridine into the fluorination kettle (about 2300kg), put the catalyst antimony pentafluoride 200kg into the reaction fluorine, add 1700kg of anhydrous hydrogen fluoride, press 2,3 - The molar ratio of dichloro-5-trichloromethylpyridine to hydrogen fluoride is 1:11, and excess hydrogen fluoride is beneficia...

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Abstract

The invention relates to the technical field of chemical synthesis, and in particular discloses a preparation method of 2-fluorine-3-chlorine-5-trifluoromethylpyridine. The preparation method of the 2-fluorine-3-chlorine-5-trifluoromethylpyridine is characterized by comprising the following steps: taking 2-chlorine-5-trichloromethylpyridine as a raw material, taking tungsten hexachloride as a catalyst, heating and introducing chlorine to perform chlorination reaction, thereby obtaining 2,3-dichloro-5-trichloromethylpyridine; putting the 2,3-dichloro-5-trichloromethylpyridine into a fluorination kettle, adding antimony pentafluoride and anhydrous hydrogen fluoride, stirring and heating to perform reaction, cooling after reaction, washing with water, layering, feeding to a rectification kettle, and performing reduced-pressure rectification, thereby preparing the 2-fluorine-3-chlorine-5-trifluoromethylpyridine. The process is reliable, the raw materials are sufficient in the market and easily available, and the preparation method of the 2-fluorine-3-chlorine-5-trifluoromethylpyridine is low in production cost, simple in operation, high in yield and favorable for large-scale production.

Description

(1) Technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of 2-fluoro-3-chloro-5-trifluoromethylpyridine. (2) Background technology [0002] Fluorine-containing compounds have the characteristics of high membrane permeability, anti-metabolism stability, affinity with lipid membranes, thermal stability and chemical stability, etc., and have been widely used in pesticides. Fluorine-containing pesticides are very important fluorine-containing fine chemicals. It has the characteristics of high selectivity, high adaptability and broad spectrum, high added value, low dosage, low cost, low toxicity, low residue, and environmental friendliness. It is in line with the development trend of modern pesticides. In the past 10 years, fluorine-containing pesticides have been developed rapidly at home and abroad. . At present, among the more than 1,300 pesticide varieties in the world, fluorine-containing pesticides...

Claims

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Application Information

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IPC IPC(8): C07D213/61
CPCC07D213/61
Inventor 肖才根刘树文
Owner SHANDONG HUIMENG BIO TECH CO LTD
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