Method for synthesizing 2,3-dichloro-5-trichloromethyl pyridine

A technology of trichloromethylpyridine and chloromethylpyridine, applied in the field of halogenation reaction, can solve problems such as lack of yield, and achieve the effects of easy operation, avoidance of waste, and convenient post-processing

Inactive Publication Date: 2015-04-22
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, there is a lack of a synthetic method

Method used

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  • Method for synthesizing 2,3-dichloro-5-trichloromethyl pyridine
  • Method for synthesizing 2,3-dichloro-5-trichloromethyl pyridine

Examples

Experimental program
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Embodiment 1

[0029] During the experiment, the reaction temperature is explored, and the screening is usually carried out by continuously increasing the range of 10-15°C.

[0030] Under the condition of 1 atmospheric pressure, after heating 20 grams of 2-chloro-5-chloromethylpyridine (0.12mol) and 0.5 gram of manganese dioxide and 0.5 gram of ferric trichloride to 120 ° C, the mixture is fed with chlorine gas The time is 45h. Using GC-MS tracking detection, it was found that 36% of the raw material was converted into 2,3-dichloro-5-trichloromethylpyridine. When the temperature of the reaction system was heated to 170° C., chlorine gas was continued to be introduced for 7 h, and GC-MS tracking detection revealed that the raw materials had reacted completely. The reaction mixture was diluted with n-hexane, washed with aqueous sodium carbonate, the organic layer was separated, dried over anhydrous sodium sulfate and the solvent was removed by distillation to obtain 25.4 g of yellow liquid 2,...

Embodiment 2

[0032] The difference with Example 1 is: under the condition of 10 atmospheric pressure, to 2-chloro-5-chloromethylpyridine 162 grams (1mol) and ruthenium trichloride 4 grams (2.5W.t%), 4 grams MoCl O (2.5 W.t%) slowly feed 473 grams of chlorine into the mixture, all of which are heated to 175°C to 180°C, after 25h, the reaction mixture is cooled, and diluted with carbon tetrachloride to separate the organic phase, washed with sodium carbonate solution, and washed with anhydrous Na2SO4 dried. The solvent was evaporated to obtain 223 g of yellow oily liquid 2,3-dichloro-5-trichloromethylpyridine with a yield of 84%.

Embodiment 3

[0034] The difference with Example 1 is: under the condition of 6 atmospheric pressure, react under the condition of 170 ℃ with 40 grams of 2-chloro-5-chloromethylpyridine and 2.0 grams (5W.t%) catalyst cobalt dichloride After 16 hours, the product was post-treated to obtain 50 g of yellow liquid 2,3-dichloro-5-trichloromethylpyridine with a yield of 76%.

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Abstract

The invention discloses a method for synthesizing 2,3-dichloro-5-trichloromethyl pyridine. The method comprises the following steps: heating 2-chloro-5-chloromethylpyridine as a raw material to reaction temperature of 70-280 DEG C, at 1-10 atmospheric pressure, in the presence of a catalyst, carrying out chlorination reaction on 2-chloro-5-chloromethylpyridine and chlorine and filtering to obtain 2,3-dichloro-5-trichloromethyl pyridine, wherein the catalyst is one or a combination of more selected from ferric chloride, ruthenium trichloride, cobalt dichloride and hexacarbonyl molybdenum. The method has the advantages of cheap raw material and higher purity and yield, and is simple in operation and convenient for after-treatment, and the large-scale industrial production can be performed.

Description

technical field [0001] The invention relates to the technical field of halogenation reaction in organic synthesis, in particular to a synthesis method of 2,3-dichloro-5-trichloromethylpyridine. Background technique [0002] 2,3-Dichloro-5-trichloromethylpyridine is an important intermediate of pesticide and medicine. 2,3-Dichloro-5-trichloromethylpyridine is a known compound that can be synthesized by various routes. 2,3-Dichloro-5-trichloromethylpyridine is a crucial intermediate for the preparation of high-efficiency pesticides such as haloxyfop, imidacloprid and future chlorinated pyridines. Compared with other chloropyridine derivatives, 2,3-dichloro-5-trichloromethylpyridine is an intermediate with particularly outstanding performance in the preparation of herbicides and insecticides. It has the remarkable characteristics of high efficiency and low toxicity, and has a wide range of applications and broad market prospects. [0003] Catalyst activity may depend to a la...

Claims

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Application Information

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IPC IPC(8): C07D213/61
CPCC07D213/61
Inventor 金朝俊于梦轩袁宇
Owner YANGZHOU UNIV
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