Preparation method of N,N-dimethyl benzamide

Abstract

The invention relates to a preparation method of N,N-dimethyl benzamide. The preparation method comprises the following steps: sequentially adding dibenzoyl methane, iodosobenzene, N,N-dimethyl formamide solution and one No.5 magneton into a reaction tube, putting the reaction tube into an oil bath pan at the temperature of 25 DEG C, heating, carrying out magnetic stirring and reacting for 24 hours, after reaction is finished, pouring reaction liquid into a separatory funnel, adding ethyl acetate, so that an organic solvent is dissolved into ethyl acetate, carrying out reverse extraction for three times with 15mL distilled water, collecting an organic phase, and then carrying out reduced pressure distillation, so that a crude product is obtained, and carrying out column chromatographic separation on the obtained crude product, so that light yellow N,N-dimethyl benzamide is obtained. The preparation method provided by the invention has the advantages that reaction conditions are mild, selectivity is high, no metal catalyst is adopted, yield is relatively high, and environmental friendliness is realized. Detection shows that the synthesized N,N-dimethyl benzamide has bioactivity andcan be applied to the fields of drug synthesis, pesticide synthesis and coating and dye synthesis.

Description

technical field [0001] The invention relates to a preparation method for synthesizing N,N-dimethylbenzamide without metal catalysis. Background technique [0002] As an important structural unit, amides widely exist in natural products, drugs, polymers and proteins. Amide compounds play an important role in many fields such as pharmaceutical industry, material chemistry and biochemistry. Research shows that more than a quarter of drugs are amides. Many important natural products, such as proteins, polypeptides, and enzymes that maintain various daily lives of organisms, contain a large number of amide bonds. In addition, widely used polymer materials, such as nylon, are also polyamide polymers composed of a large number of amide bonds. Among them, aryl-containing amides are an important class of compounds. [0003] There are many methods for the synthesis of aromatic amides. The earliest aromatic amidation reaction is the arylation reaction catalyzed by copper. However, t...

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Problems solved by technology

[0003] There are many methods for the synthesis of aromatic amides. The earliest aromatic amidation reaction is the arylation reaction catalyzed by copper. However, this method is limited to the coupling between halogenated aromatic hydrocarbons and aromatic amides, and an excessive amount of Copper powder, the reaction temperature is higher, exceeding 200 ° C. Later, Buchwald et al. used ethylenediamine as a ligand, and the Goldberg reaction catalyzed by CuI can be carried out under milder conditions

Since then, studies have found that under the conditions of Pd, Ni, Cu, etc. as catalysts, halogenated aromatic hydrocarbons, benzyl alcohol, aldehydes, etc. react with various (amide) amides to obtain the corresponding aromatic amides. These reactions broaden the reaction base. The types of substances increase the diversity of reactions, and the tolerance of reactive functional groups is better. However, one or more expensive metals will be used as auxiliary reagents for the reaction in these reaction catalytic systems, and phosphorus oxychloride, Phosphine ligands, additives, auxiliary agents and other toxic and harmful substances

With the strengthening of people's awareness of environmental protection and the current development trend of green, efficient and economical chemical reactions, the reaction conditions of this type of reaction need to be improved.

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