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Preparation method of 2-chlorin-6-trifluoro picoline

A technology of trifluoromethylpyridine and picoline, applied in the field of preparation of pesticide intermediate 2-chloro-6-trifluoromethylpyridine, which can solve the problems of difficult separation of tar, low product purity, and difficult equipment , to achieve the effect of low production cost, high purity and easy operation

Inactive Publication Date: 2007-12-05
山东广恒化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Only 35% of the product is produced, there are many by-products, tar is difficult to separate, the product is low in purity, and it is difficult to solve it with other equipment

Method used

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  • Preparation method of 2-chlorin-6-trifluoro picoline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Chlorination

[0029] Pump into the 1000L chlorination kettle 200kg of dried raw materials 2-chloro-6-methylpyridine, 6kg of phosphorus trichloride, 1000kg of carbon tetrachloride, 5kg of benzoyl peroxide, and turn on the light source (800W ultraviolet light) Two), the jacket is ventilated to increase the temperature, the tail gas system is turned on, and the micro-negative pressure (-0.01MPa) is operated. When the temperature in the kettle reaches 80℃, the chlorine will be ventilated. The chlorine vent is 45kg / h, first fast and then slow. Keep the reflux reaction. Through sampling and analysis, GC detects that the trichloride content is above 90% and the dichloride is less than 5% as the end of the reaction. If the reaction needs to continue, sampling and analysis will be performed every 2 hours until it is qualified.

[0030] After qualified, stop the chlorine flow, pump the reaction liquid into the carbon tetrachloride distillation kettle, and distill the carbon tetr...

Embodiment 2

[0037] The same process steps as in Example 1. The different conditions are:

[0038] The catalyst used in the chlorination reaction stage is 15 kg of benzoyl peroxide. The organic solvent uses 1,200 kg of trichloromethane.

[0039] In the fluorination reaction stage, the catalyst antimony pentachloride is used, the addition amount is 1kg, the reaction temperature is 170-180°C, and the pressure is 7Mpa, and the reaction time is 24 hours.

[0040] The purity of the product is over 98%, and the yield is 85%.

Embodiment 3

[0042] The same process steps as in Example 1. The different conditions are:

[0043] The catalyst used in the chlorination reaction stage is 7 kg of tungsten hexachloride and 3 kg of phosphorus trichloride.

[0044] The organic solvent is 2000kg of nitrobenzene.

[0045] In the fluorination reaction stage, the catalyst antimony pentafluoride is used, the added amount is 0.7kg, the reaction temperature is 170-180°C, the pressure is 8Mpa, and the reaction time is 27 hours.

[0046] The purity of the product is over 98%, and the yield is 86%.

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Abstract

The process of preparing 2-chloro-6-trifluoromethylpyridine as one new type of pesticide intermediate includes the following steps: chloridizing 2-chloro-6-tetramethyl pyridine in refluxing organic solvent, eliminating organic solvent, heating to dissolving chloridizing material, fluorinating, steam distilling, separating and rectifying. The process of the present invention is simple, easy to operate and favorable to industrial production, and the obtained product has purity not lower than 98 %, yield of 85 % and low production cost.

Description

Technical field [0001] The invention relates to a preparation method of pesticide intermediate 2-chloro-6-trifluoromethylpyridine. Background technique [0002] 2-Chloro-6-trifluoromethylpyridine is a key intermediate in the synthesis of insecticides. Insecticides were successfully developed by a US company in the 1990s to control pests in field crops such as cotton, soybeans, and rape. It has the characteristics of strong medicinal effect, small dosage per mu, low toxicity, low residue, and remarkable effect. It is the backbone product that has been upgraded to insecticide in foreign developed countries. [0003] 2-Chloro-6-trifluoromethylpyridine is not only used as a new pesticide intermediate, but also has a wide range of uses in the fields of organic synthesis, dyes and medicine. In recent years, it has been found that the introduction of trifluoromethyl on the heterocycle can increase the affinity of the compound. Lipidity, thereby improving the permeability of biological m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/61
Inventor 王彬
Owner 山东广恒化工有限公司
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