Method for efficient solid-phase synthesis of amide derivative through carboxylic acid and urea

Abstract

The invention discloses a method for efficient solid-phase synthesis of an amide derivative through carboxylic acid and urea. The method comprises the steps that a carboxylic acid and urea mixture anda catalyst are mixed, a mixture is placed in a sealed pipe of a single-mode microwave device and heated, then through a monitoring reaction endpoint, namely the ratio, being 4:1, of cyclohexane to ethyl acetate in thin-layer chromatography (TLC), reactants are cooled to the room temperature, extraction is conducted through the ethyl acetate, then an extract is sequentially washed by hydrochloricacid, a sodium bicarbonate solution and water, an organic layer is dried by anhydrous magnesium sulfate, a solvent is subjected to decompressed distillation, and thus the amide derivative is obtained.Benzoic acid and the urea are mixed and heated for a long time at 220 DEG C, a chemical reaction can be completed only within 20-80 seconds by applying a microwave assistive technology, and the effect higher than the effect achieved by conventional heating is achieved. By applying a solvent-free solid phase method and utilizing an easy-to-obtain reagent, high-yield amide is prepared through a simple and effective method, and the solvent-free solid phase method has the advantages of high reaction speed, low catalyst cost and the like.

Description

technical field [0001] The invention relates to the technical field of preparation of amide functional groups, in particular to a method for efficiently solid-phase synthesis of amide derivatives from carboxylic acid and urea. Background technique [0002] The amide functional group is an important unit in naturally occurring or synthetic organic molecules. The amide bond is a negatively charged functional group. In organic chemistry, the chemical formula of the amide bond is -CO-NH-, in which carbon and oxygen form a double bond, and nitrogen and hydrogen form a single bond. In biochemistry, an amide bond refers to a peptide bond, which is formed by the dehydration condensation of the amino group of one molecule of amino acid and the carboxyl group of another molecule of amino acid, that is, at least two or more amino acids are required to form a peptide bond, so only dipeptides and polypeptides The amide bond is called a peptide bond. [0003] There are several protocols...

AI Technical Summary

Problems solved by technology

However, in most cases, either complex or expensive reagents are involved, or the reaction takes a long time, or uses corrosive reagents and a large amount of solid supports, and eventually produces a large amount of toxic waste polluting the environment

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