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2-chloro-5-tirfluoromethylpyridine and synthetic method thereof

A technology of trifluoromethylpyridine and a synthesis method, applied in directions such as organic chemistry, can solve problems such as expensive catalyst manganese fluoride, ozone layer destruction by carbon tetrachloride, consumption of hydrofluoric acid, etc., and achieve low cost and production cost. Low, reduce the effect of intermediate links

Active Publication Date: 2013-01-16
潍坊新绿化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Its shortcomings are: (1) the catalyst manganese fluoride is expensive; (2) the carbon tetrachloride used has damage to the ozone layer and has a great impact on the environment, and under the process conditions, carbon tetrachloride will react with hydrofluoric acid The reaction consumes part of the hydrofluoric acid, resulting in a large number of by-products

Method used

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  • 2-chloro-5-tirfluoromethylpyridine and synthetic method thereof
  • 2-chloro-5-tirfluoromethylpyridine and synthetic method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Such as figure 1 As shown, 2.5% CoCl by mass is charged in the reaction tube 3 2 / C 40g. After the temperature of reaction tube 3 rises to 380°C, chlorine gas and HF are introduced, wherein the chlorine gas flow rate is kept at 5 L / h, and the HF flow rate is kept at 10 L / h. Chlorine gas and HF are introduced for 1 hour (the purpose is to activate the catalyst). The vaporizer 1 and the reaction tube 3 are respectively heated by two heating furnaces 2 .

[0029] Pass 3-picoline into vaporizer 1 for vaporization, the temperature of vaporizer 1 is 250°C, and nitrogen gas is introduced at the same time to bring the vaporized 3-picoline into reaction tube 3 after the catalyst has been activated, where 3-methylpyridine The flow rate of pyridine is maintained at 5g / h, and the flow rate of nitrogen gas is maintained at 15L / h;

[0030] During the reaction process, 3-picoline, chlorine, HF and nitrogen maintain the original flow rate, and the tail gas leaving the reaction tube ...

Embodiment 2

[0033] Load the mass percent 2.8%CoCl in the reaction tube 2 / C 40g. After the temperature of the reaction tube rose to 380°C, chlorine gas and HF were introduced, wherein the chlorine gas flow rate was maintained at 5 L / h, and the HF flow rate was maintained at 10 L / h. Chlorine gas and HF gas were introduced for 1 hour (the purpose was to activate the catalyst).

[0034] Pass 3-picoline into the vaporizer to vaporize, the temperature of the vaporizer is 250°C, and at the same time pass nitrogen to bring the vaporized 3-picoline into the reaction tube after the catalyst has been activated, and the flow rate of 3-picoline Keep at 5g / h, nitrogen flow rate at 15L / h;

[0035] During the reaction process, 3-picoline, chlorine, HF and nitrogen maintain the original flow rate, and the tail gas leaving the reaction tube is condensed to obtain an oil, and the composition of the product is analyzed by conventional chromatographic methods. Among them, 2-chloro-5-trifluoromethylpyridine...

Embodiment 3

[0038] Load the mass percentage 3.5%CoCl in the reaction tube 2 / C 40g. After the temperature of the reaction tube rose to 380°C, chlorine gas and HF were introduced, and the chlorine gas flow rate was maintained at 5 L / h, and the HF flow rate was maintained at 10 L / h. Chlorine gas and HF gas were introduced for 1 hour (the purpose is to activate the catalyst).

[0039] Pass 3-picoline into the vaporizer to vaporize, the temperature of the vaporizer is 250°C, and at the same time pass nitrogen to bring the vaporized 3-picoline into the reaction tube after the catalyst has been activated, and the flow rate of 3-picoline Keep at 5g / h, nitrogen flow rate at 15L / h;

[0040] During the reaction process, 3-picoline, chlorine, HF and nitrogen were kept at the original flow rate, and the tail gas leaving the reaction tube was condensed to obtain an oil, and the composition of the product was analyzed by conventional chromatographic methods. Among them, 2-chloro-5-trifluoromethylpyri...

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Abstract

The invention discloses a 2-chloro-5-tirfluoromethylpyridine and a synthetic method thereof. The synthetic method of the 2-chloro-5-trifluoromethylpyridine comprises the following steps of: (1) feeding 3-methylpyridine into a vaporizer to vaporize the 3-methylpyridine; (2) adding a catalyst into a reactor and heating the reactor to a reaction temperature, and feeding chlorine gas and hydrogen fluoride gas into the reactor; and (3) by utilizing nitrogen as a carrier gas, carrying the vaporized 3-methylpyridine into the reactor so as to be subjected to reaction, and condensing, purifying and separating the gas after reaction, so that 2-chloro-5-trifluoromethylpyridine and 2-chloro-3-trifluoromethylpyridine are obtained. According to the synthetic method disclosed by the invention, the cobalt dichloride catalyst is available and is lower in price, industrialization is easy to realize, catalytic selectivity to two target products is high, and the yield is high; and nitrogen is adopted as the carrier gas, and the nitrogen is available, low in cost and safer and has less possibility of influencing the environment, so that the synthetic method disclosed by the invention is beneficial to industrial production.

Description

technical field [0001] The invention relates to a synthetic method for preparing 2-chloro-5-trifluoromethylpyridine and 2-chloro-3-trifluoromethylpyridine by chlorofluorination of 3-picoline. Background technique [0002] Both 2-chloro-5-trifluoromethylpyridine and 2-chloro-3-trifluoromethylpyridine are important pyridine chemical raw materials. 2-Chloro-5-trifluoromethylpyridine can synthesize many compounds with special uses, and is an important intermediate suitable for medicine and agricultural chemicals. Key intermediates of pesticides such as chrysanthemum and fungicide fluazinam. 2-Chloro-3-trifluoromethylpyridine is the key intermediate for the production of the high-efficiency herbicide rimsulfuron-methyl, and it is also the intermediate for the synthesis of nicosulfuron-methyl by hydrolysis into 2-chloronicotinic acid. It can be seen that it has a wide range of uses. The method for synthesizing 2-chloro-5-trifluoromethylpyridine includes by raw material classific...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/61
Inventor 魏礼超李学武王通善崔卫涛杨洪强朱恒营
Owner 潍坊新绿化工有限公司
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