Synthesis method of 2, 3-dichloro-5-trichloromethylpyridine

A technology of trichloromethylpyridine and synthesis method, which is applied in the field of synthesis of 2,3-dichloro-5-trichloromethylpyridine, and can solve the problems of difficult post-processing, low utilization rate of chlorine gas, long chlorination time, etc. , to achieve a significant effect of chlorination

Inactive Publication Date: 2021-06-11
JIANGSU YOUJIA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The purpose of the present invention is to provide a synthetic method of 2,3-dichloro-5-trichloromethylpyridine, which overcomes the high chlorination temperature, long chlorination time, low chlorine utilization rate and product Technical defects such as difficult post-processing, the total yield of 2,3-dichloro-5-trichloromethylpyridine is 82-93%

Method used

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  • Synthesis method of 2, 3-dichloro-5-trichloromethylpyridine
  • Synthesis method of 2, 3-dichloro-5-trichloromethylpyridine

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Embodiment 1

[0038] A kind of synthetic method of 2,3-dichloro-5-trichloromethylpyridine, comprises the following steps:

[0039] (1) Weigh 1.0g of ferric chloride in a flask, measure 100mL of deionized water, weigh 10g of activated carbon carrier and slowly add it to the flask, stir for 30min, ultrasonically disperse for 20min, soak at 60°C for 12h, and then put it in an oven at 120°C Dry for 12 hours, pass through a 200-mesh sieve after grinding, and put into a resistance furnace N 2 Roasting at 160°C for 4 hours under protection to obtain catalyst B supported by activated carbon;

[0040] Fill 1.0g of Catalyst B into the second half of the channel of the microreactor, and compact it with a microporous partition; after connecting the primary chlorination and secondary chlorination micro-reaction channels in series, connect the mixing chamber to the preheating chamber, and The heat chamber is connected to the channel inlet I of the microreactor, the channel inlet II of the microreactor i...

Embodiment 2

[0045] A kind of synthetic method of 2,3-dichloro-5-trichloromethylpyridine, comprises the following steps:

[0046] (1) Weigh 1.0g of ruthenium trichloride in a flask, measure 100mL of ionized water, weigh 10g of activated carbon carrier and slowly add it to the flask, stir for 30min, ultrasonically disperse for 20min, soak at 60°C for 12h, and then dry in an oven at 120°C 12h, pass through a 200-mesh sieve after grinding, and put it into a resistance furnace N 2 Roasting at 160°C for 4 hours under protection to obtain catalyst B supported by activated carbon;

[0047] Fill 1.0g of Catalyst B into the second half of the channel of the microreactor, and compact it with a microporous partition; connect the primary chlorination and secondary chlorination micro-reaction channels in series, and then connect the mixing chamber to the preheating chamber, The preheating chamber is connected to the channel inlet I of the microreactor, the channel inlet II of the microreactor is conne...

Embodiment 3

[0052] A kind of synthetic method of 2,3-dichloro-5-trichloromethylpyridine, comprises the following steps:

[0053] (1) Weigh 1.0g of tungsten hexachloride in a flask, measure 100mL of ionized water, weigh 10g of activated carbon carrier and slowly add it to the flask, stir for 30min, ultrasonically disperse for 20min, soak at 60°C for 12h, and then dry in an oven at 120°C 12h, pass through a 200-mesh sieve after grinding, and put it into a resistance furnace N 2 Roasting at 160°C for 4 hours under protection to obtain catalyst B supported by activated carbon;

[0054] Fill the second half of the microreactor channel with 1.0g of catalyst B, and compact it with a microporous partition; connect the primary chlorination and secondary chlorination microreaction channels in series, then connect the mixing chamber to the preheating chamber, and preheat The heat chamber is connected to the channel inlet I of the microreactor, the channel inlet II of the microreactor is connected t...

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Abstract

The invention discloses a synthesis method of 2, 3-dichloro-5-trichloromethylpyridine, which is characterized in that a microreactor is used as a chlorination reaction channel, the first half of the microreactor channel is used as a primary chlorination channel, and the second half of the microreactor channel is filled with a catalyst B as a secondary chlorination reaction channel. The method comprises the following steps of firstly, fully mixing 2-chloro-5-methylpyridine with a catalyst A in a mixing chamber, then continuously reacting with chlorine through a primary chlorination channel to obtain 2-chloro-5-trichloromethylpyridine, then reacting through a secondary chlorination channel to obtain a crude oil layer of 2, 3-dichloro-5-trichloromethylpyridine, and carrying out alkali washing, dechlorination and rectification on the crude oil layer to obtain the high-concentration 2, 3 -dichloro-5-trichloromethylpyridine with the total yield to be 82-93%. According to the method, the technological process is simple, amplification production can be carried out through parallel connection, the catalyst B can be recycled and reused, the chlorination time is remarkably shortened, the chlorine utilization rate is increased, the post-treatment difficulty of the product is reduced, and the synthesis cost of 2, 3-dichloro-5-trichloromethylpyridine is saved.

Description

technical field [0001] The invention relates to a synthesis method of 2,3-dichloro-5-trichloromethylpyridine, in particular to using 2-chloro-5-methylpyridine as a raw material, using a microchannel reactor to undergo primary chlorination and secondary Chlorination reaction to synthesize 2,3-dichloro-5-trichloromethylpyridine. Background technique [0002] 2,3-Dichloro-5-trichloromethylpyridine is an important pesticide intermediate. It is not only used in the synthesis of the pesticide nitenpyram, but also an important component of the neonicotinoid pesticides imidacloprid, acetamiprid, and thiacloprid. intermediate. Its downstream product 2,3-dichloro-5-trifluoromethylpyridine is an important intermediate in fluorinated nitrogen heterocyclic pesticides. Fluorine-containing herbicides such as haloxyfop and haloxyfop have the characteristics of high efficacy, low toxicity, and small pollution. Another class of fluorine-containing benzoylurea insecticides, such as difluzur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/61B01J19/00
CPCC07D213/61B01J19/0093Y02P20/584
Inventor 吴孝举孔勇李志峰谢邦伟冯素流张斌孙荣杰
Owner JIANGSU YOUJIA CHEM
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