Method for synthesizing 2,3í»-dichloroacetophenone

A technology of dichloroacetophenone and chloroacetophenone, applied in 2 fields, can solve problems such as difficult and difficult to carry out

Inactive Publication Date: 2008-12-31
徐州诺特化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

The α-halogenation of m-chloroacetophenone is also a relatively difficult reaction, because the α-halogenated product is easy to polymerize, and it is directly obtained by chlorine or bromine, and it is not easy to carry out

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment Construction

[0008] The present invention will be further described below in conjunction with specific examples, but the present invention is not limited to these specific examples.

[0009] Example 1:

[0010] Preparation of m-chloroacetophenone: Cool 60ml of concentrated hydrochloric acid, 60ml of water and 23g of m-aminoacetophenone with ice-salt water to 0-5°C, then add dropwise under stirring solution (under the liquid surface), and keep the reaction temperature 0 ~ 5 ℃, dropwise, continue to react for 20min. Pour the above-prepared diazonium salt solution into cold CuCl hydrochloric acid solution (17g CuCl+55ml concentrated hydrochloric acid), heat to 50-60°C, stir well and let stand for 2-3 hours. The solid material and the aqueous phase were separated to give an oil. The oil was washed with water until the aqueous solution was neutral. The oil was added to water and distilled with steam until there was no oil drop. The oil layer was separated, and the water layer was extracted ...

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Abstract

The invention relates to a synthesis method for 2,3'-dichloroacetophenone (alpha-chloro-acetophenone inter-chlorophenyl) and is characterized in that the method takes inter-amino-acetophenone as raw material to generate between inter-acetophenone diazo-hydrochloride through diazotization reaction, or generate inter-p-acetophenone through Sandmeyer reaction, or generate 2,3'-dichloroacetophenone through alpha-chloro-reaction; the synthetic way is simple and the conditions are mild, with a total yield rate more than 80%.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and relates to a method for organic synthesis of 2,3'-dichloroacetophenone. Background technique [0002] 2,3'-Dichloroacetophenone is an important organic raw material, which can be used to synthesize pharmaceutical raw materials and other organic compounds. Generate m-chloroacetophenone by acetophenone, can adopt acetophenone in carbon tetrachloride solvent, under iron trichloride as catalyst, generate with chlorine gas substitution reaction, but this reaction simultaneously generates ortho and meta Chloroacetophenones. The separation of the reaction mixture usually adopts the vacuum distillation method, and its separation effect is not good, and it is difficult to obtain m-chloroacetophenone with a content of 99%. Adopt aluminum chloride catalyst, in acetic acid or chlorobenzene solvent, chlorobenzene and acetyl chloride take place Friedel-Crafts reaction, can only generate p-chlor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/80C07C45/63
Inventor 王玉成胡晓高玉忠王理想王友志杨凯曹再林张春来张文娟靳长娟徐安民王乃剑
Owner 徐州诺特化工有限公司
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