41176-98-1Relevant academic research and scientific papers
Preparation method of glimepiride impurity
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, (2020/04/02)
The invention belongs to the technical field of medicinal chemistry and particularly relates to a preparation method of a glimepiride impurity. The preparation method comprises the following steps: dropwise adding acetic anhydride into a solution of 2-phenethylamine and an organic solvent with a low boiling point to be subjected to reaction to generate N-acetyl phenethylamine; dropwise adding chlorosulfonic acid into the N-acetyl phenethylamine at the temperature of lower than 20 DEG C to be subjected to chlorosulfonation reaction, and performing hydrolysis after the reaction is completed to remove excess chlorosulfonic acid; performing filtration and washing to obtain an impurity J benzenesulfonyl chloride; performing ammonolysis on the impurity J benzenesulfonyl chloride to obtain an impurity J benzene sulfonamide; in acetone, enabling the impurity J benzene sulfonamide to firstly react with a catalyst and then react with trans-p-methylcyclohexyl isocyanate to obtain an impurity J acetyl substance; enabling the impurity J acetyl substance and ethanol to be subjected to alcoholysis under the condition of the catalyst to generate an impurity J and ethyl acetate; and performing refining to obtain a high-purity impurity J. The purity of the glimepiride impurity J prepared by the method is high, the liquid phase content of the glimepiride impurity J is greater than 98.5%, the rawmaterials used in the method are easily available, the process parameters are controllable, and the reaction is mild.
