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Combined preparation method of 2-cyano-3-chloro-5-trifluoromethylpyridine and succinonitrile

A technology of trifluoromethyl pyridine and combined preparation, which is applied in cyanide reaction preparation, carboxylic acid nitrile purification/separation, organic chemistry and other directions, can solve the problems of large amount of waste water and difficult treatment, and achieves less waste water and easy treatment. , Easy to recycle and apply

Inactive Publication Date: 2021-02-23
内蒙古佳瑞米精细化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to overcome the large amount of existing process wastewater and the problem that it is difficult to handle, the invention provides a joint preparation method of 2-cyano-3-chloro-5-trifluoromethylpyridine and succinonitrile, excessive potassium cyanide / All sodium is consumed by dichloroethane or dibromoethane

Method used

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  • Combined preparation method of 2-cyano-3-chloro-5-trifluoromethylpyridine and succinonitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027](98%) (98%) of potassium pelicide particles 132.5 g (1.995 mol) and 300 g (16.7 mol) were added, stirred until completely dissolved. Further, 4-dimethylaminopyridine 3.7 g (0.025 mol), 394.8 g (3.989 mol) and 2-fluoro-3-chloro-5-trifluoromethylpyridine 200g (0.997 mol) were added.

[0028]Then the stirring was evenly stirred to a reflux reaction for 12 h, and the temperature of the reaction liquid is 0.2 ppm, the reaction liquid is lowered to 30-35 ° C, and the lower layer is the product mixture (the aqueous layer is added. After the chloroethane, stir, stand in the layers, and the dichloroethane layer is used for the next batch reaction). The product mixed was mixed with dichloroethane at normal pressure to prepare dichloroethane 285 g. Then the pamiditrile was minipitricile at 3 kPa vacuum to give 66.0 g of butidonitrile, and the content was 99.9%. Dikinonitrile and 2-cyano-3 chloro-5-trifluoromethylpyridine transition fraction 22.3g analysis of butonlonitrile content 41.3%, 2-...

Embodiment 2

[0030]Under the conditions of room temperature, (98%) of (98%) of potassium particles 132.5 g (1.995 mol) and 300 g (16.7 mol) were added, stirred until completely dissolved in a 1000 ml of tetra-mouth flask. The benzyl triethyl chloride was added 5.7 g (0.025 mol), 394.8 g (3.989 mol) and 2-fluoro-3-chloro-5-trifluoromethylpyridine (0.997 mol).

[0031]Then the stirring was mixed and then raised to 75-78 ° C for refluxing reaction for 10 h, and the temperature of the reaction liquid is 0.2 ppm, and the reaction liquid is lowered to 30-35 ° C, stand in the layered, the lower layer is a product mixture (the aqueous layer added to the second After the chloroethane, stir, stand in the layers, and the dichloroethane layer is used for the next batch reaction). The product mixture was mixed with dichloroacethane atmospheric pressure, and then pamiditrile was minimalized at 3 kPa vacuum to give 68.3 g of butidonitrile, the content was 99.9%. Dikinnitrile and 2-cyano-3-chloro-5-trifluoromethyl...

Embodiment 3

[0033](98%) (98%) of potassium pelicide particles 132.5 g (1.995 mol) and 300 g (16.7 mol) were added, stirred until completely dissolved. Further, 4-dimethylaminopyridine 3.7 g (0.025 mol) was added, and 394.8 g (3.989 mol) and 2-fluoro-3-chloro-5-trifluoromethylpyridine (0.997 mol) were recovered. .

[0034]Then the stirring was evenly stirred to a reflux reaction for 12 h, and the temperature of the reaction liquid is 0.2 ppm, the reaction liquid is lowered to 30-35 ° C, and the lower layer is the product mixture (the aqueous layer is added. After the chloroethane, stir, stand in the layers, and the dichloroethane layer is used for the next batch reaction). The product mixture was distilled at normal pressure to collect dichloroethane to recover dichloroethane. The transition fraction obtained in Example 1 was then 22.3 g (41.3% butbitonitrile content of 41.3%, 2-cyano-3-chloro-5-trifluoromethylpyridine) was added to the distillation tank. Diatronerconitrile was mining at 3 kPa vacu...

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Abstract

The invention discloses a combined preparation method of 2-cyano-3-chloro-5-trifluoromethylpyridine and succinonitrile, and belongs to the field of organic chemistry. The method comprises the following steps: taking 2-fluoro-3-chloro-5-trifluoromethylpyridine and dichloroethane as raw materials, reacting in a potassium cyanide / sodium solution under the action of a phase transfer catalyst to obtaina mixed solution of 2-cyano-3-chloro-5-trifluoromethylpyridine and succinonitrile, layering, washing with water, and rectifying to obtain the 2-cyano-3-chloro-5-trifluoromethylpyridine with the content of more than 99% and the succinonitrile with the content of more than 99.9%. According to the method, the yield is high, the wastewater treatment is simple, byproducts are fully utilized, the yieldof the 2-cyano-3-chloro-5-trifluoromethylpyridine can reach 93%, and the yield of the succinonitrile can reach 95%.

Description

Technical field[0001]The present invention belongs to the field of organic chemistry, and more particularly to a combination of 2-cyano-3 chloro-5-trifluoromethylpyridine and butadonitrile.[0002]technical background[0003]2-cyano-3-chloro-5-trifluoromethylpyridine is an important pesticide intermediate, mainly used to produce 2-methyl amino-3-chloro-5-trifluoromethylpyridine hydrochloride, fluorine Pesticide chemical products such as ether bacteria. Dikaitrile is an important pharmaceutical intermediate, or it can also be used to produce automotive coatings, battery additives, etc.[0004]Foreign patents react with 4-dimethyl-5-trifluoromethylpyridine as the raw material, and then react with cyanide or cyanide, sodium cyanide or cyanide after crystalline drying. 2-cyano-3 chloro-5-trifluoromethylpyridine was distilled, and the yield was 80%. The operation process is cumbersome, low yield, and the resulting cyanide waste water is extremely large, treated and difficult, is not conducive ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/84C07C253/14C07C253/34C07C255/09
CPCC07C253/14C07C253/34C07D213/84C07C255/09
Inventor 张海东向彬李君刚宏辉柯有胜
Owner 内蒙古佳瑞米精细化工有限公司
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