Electrochemical preparation method of beta-trifluoromethylamide compounds

A technology of trifluoromethyl amide and trifluoromethyl, which is applied in the direction of electrodes, electrolysis process, electrolysis components, etc., can solve the problems of cumbersome preparation steps of three-step methylation reagents, expensive photocatalytic catalysts, and hindering the development of applications. , to achieve good functional group tolerance, less waste emissions, and avoid the use of catalysts

Active Publication Date: 2019-07-05
WUYI UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

However, due to the high price of photocatalytic catalysts, the high cost and cumbersome preparation steps of three-step methylation reagents have become the main factors hindering the development of related applications.

Method used

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  • Electrochemical preparation method of beta-trifluoromethylamide compounds
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  • Electrochemical preparation method of beta-trifluoromethylamide compounds

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Embodiment 1

[0025] Embodiment 1 of the present invention is: an electrochemical preparation method of β-trifluoromethyl amide compounds, comprising the following steps: using aryl acetylene compounds represented by formula (I) as raw materials, trifluoromethyl trifluoromethyl Fluorosilane is used as a source of trifluoromethyl, and by electrochemical anodic oxidation, tetra-n-butylammonium acetate is used as an electrolyte, reacted in a solvent composed of acetonitrile and ethanol for a period of time, and then purified to obtain formula (II) The β-trifluoromethylamide product shown;

[0026]

[0027] In the scheme of the present invention, with CF 3 SO 2 Na is used as a trifluoromethyl source, acetonitrile is used as both a reactant and a solvent, and a cyano group is used as an amide source to achieve trifluoromethylation of the amino group at the ortho position; trifluoromethyltrifluorosilane is used as a trifluoromethyl The base source and tetra-n-butylammonium acetate are used a...

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Abstract

The invention discloses an electrochemical preparation method of beta-trifluoromethylamide compounds. The method comprises the following step: preparing the beta-trifluoromethylamide compounds by using an aryl acetylene compound and a trifluoromethyl source as raw materials through an electrochemical anodic oxidation method. The preparation method further comprises the step of purifying the product obtained by the electrochemical anodic oxidation method, wherein the purification treatment comprises the following processes: after the reaction is completed, adding ethyl acetate for a quenching reaction, adding saturated brine, performing washing, separating the organic phase, performing extraction on the aqueous phase by using ethyl acetate for 3-5 times, merging the organic phase, adding anhydrous sodium sulfate for drying, performing reduced-pressure distillation to remove a solvent, and performing column chromatography to obtain the higher-purity beta-trifluoromethylamide compounds. Compared with the prior art, the solution provided by the invention has the advantages of simple and convenient operation, low production costs and a high yield.

Description

technical field [0001] The invention relates to the field of organic compound synthesis, in particular to a method for synthesizing β-trifluoromethylamide compounds by using aryl acetylene compounds under electrochemical oxidation conditions. Background technique [0002] Ortho-difunctionalization of alkenes has been considered as an effective strategy to rapidly and directly construct different molecular structures by introducing different groups on adjacent carbon atoms. In recent years, the ortho-trifluoromethyl functionalization of alkenes has attracted much attention, due to the introduction of CF 3 Groups can significantly change the physical, chemical and biological properties of organic molecules. Therefore, compounds containing trifluoromethyl groups are widely used in medicine, pesticides and other fields. Currently, reaction systems including transition metal catalyst systems and photoredox systems to initiate the formation of trifluoromethyl radicals by stoichio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/02C25B11/04C25B3/23
CPCC25B11/04C25B3/23
Inventor 黄玉冰卢景俊江虹李亦彪朱忠智陈修文
Owner WUYI UNIV
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