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Method for preparing 2,3 - dichloro - 5 - trichloro methylpyridine

A technology of trichloromethylpyridine and chloromethylpyridine, which is applied in the field of organic synthesis and can solve the problems of difficult industrialization, expensive catalysts, and high production costs

Active Publication Date: 2009-12-02
LANZHOU CHEMSPECWEIER CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In summary, according to the methods listed above, there are the following disadvantages: the production cost is too high, the catalyst is expensive and the raw materials are not easy to obtain, so that there are many difficulties in the realization of industrialization

Method used

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Examples

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Effect test

preparation example Construction

[0074] (2) The preparation method of the present invention reacts with cheap and a large amount of commercialized raw materials that are easy to buy in industry, the raw and auxiliary materials of this method are cheap and easy to get, the process is simple, the one-step reaction directly makes the target product, and the post-treatment is easy. , mild conditions, less environmental pollution, can produce 2,3-dichloro-5-trichloromethylpyridine with a relatively high yield, and is easy to industrialize at the same time.

[0075] (3) In a preferred embodiment of the present invention, a new catalyst, namely molybdenum oxide catalyst, is used. It is not easy to absorb moisture and be hydrolyzed, reduces the degree of corrosion to the reaction vessel, has milder reaction conditions, achieves higher yield, reduces cost, and reduces environmental pollution.

Embodiment 1

[0079] Drop into 500g (3.08mol) 2-chloro-5-chloromethylpyridine (molecular weight 162g / mol), 25g (5%wt) MoO 2 , stir well, at T 内 =175°C, feed Cl into the above solution 2 , The reaction was completed in 29 hours. The crude 2,3-dichloro-5-trichloromethylpyridine was washed, adjusted to PH=8-9, separated, dried and distilled to obtain 651 g of the product with a yield of 79.7%.

Embodiment 2

[0081] 500g (3.08mol) 2-chloro-5-chloromethylpyridine (molecular weight 162g / mol), 0.5g (0.1%wt) MoO 2 , stir well, at T 内 =100°C, feed Cl into the above solution 2 , 80 hours to complete the reaction. The crude 2,3-dichloro-5-trichloromethylpyridine was washed, subjected to pH=8-9, separated, dried, and distilled to obtain 93.2 g of the product with a yield of 11.4%.

[0082] The incompletely chlorinated product of the present invention can be recycled for recycling until the desired yield is achieved.

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Abstract

The invention belongs to the technical field of preparation methods of 2,3-dichloro-5-trichloromethylpyridine. The preparation method of 2,3-dichloro-5-trichloromethylpyridine of the present invention uses cheap and easy-to-obtain large-scale commercialized 2-chloro-5-chloromethylpyridine as raw material, in catalyst and chlorine etc. In the presence of , the reaction temperature is 100-250 ° C, and 2,3-dichloro-5-trichloromethylpyridine is synthesized by chlorination. The raw material catalyst used in the present invention has been commercialized on a large scale at home and abroad and in the world, and the price is low. The method of the invention has simple preparation process, can directly synthesize 2,3-dichloro-5-trichloromethylpyridine in one-step reaction, has high yield, and is extremely suitable for large-scale commercial production.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to the technical field of preparation methods of 2,3-dichloro-5-trichloromethylpyridine. Background technique [0002] 2,3-Dichloro-5-trichloromethylpyridine is a very valuable heterocyclic intermediate, which has been widely used in the fields of pesticides, medicines and fine chemicals. [0003] US4508907, US4555575, GC1599123 and other patent documents refer to the following synthetic methods: 2-amino-5-picoline is used as raw material to synthesize 2,3-dichloro-5-trichloro The disadvantages of picoline are: the cost of raw materials is high, and it is difficult to separate isomers after the reaction. [0004] The following method is disclosed in US4469896: take perhalogenated aldehyde and unsaturated nitrile as raw materials to synthesize 2,3-dichloro-5-trichloromethylpyridine, and its disadvantages are: raw material perhalogenated aldehyde synthesis and separation and purifica...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/61B01J23/28B01J27/10
Inventor 戴信培张京唐运宏
Owner LANZHOU CHEMSPECWEIER CHEM CO LTD
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