Microwave preparation method of etimicin sulfate

Abstract

The invention relates to a microwave preparation method of etimicin sulfate. The method comprises the following steps of a, adding methanol, gentamicin sulfate C1a, sulfuric acid and anhydrous zinc acetate into a microwave reaction kettle at room temperature, and performing stirring and dissolving; b, dropwise adding acetic anhydride in the step a for acetylation; c, performing microwave irradiation in the step b; d, carrying out dezincification treatment on an obtained reaction solution, injecting the reaction solution into a 732 strong acid cation exchange resin column, performing flushing with water until the optical rotation is zero, performing desorption with ammonia water to obtain a desorption solution of a required product, and carrying out reduced pressure concentration; e, addingtetrahydrofuran into a reaction kettle of an obtained oily substance, regulating the pH value with sulfuric acid, dropwise adding acetaldehyde at 15 DEG C, performing stirring, adding sodium borohydride, and performing stirring at room temperature; f, performing evaporating to remove a solvent, adding a sodium hydroxide aqueous solution, and performing microwave irradiation; and g, after the reaction is finished, concentrating the reaction solution, introducing a concentrated solution into a chromatographic separation column for sample loading, performing flushing with salt-free water, performing desorption with an ethanol aqueous solution, collecting effective components, performing concentrating, and performing refining and drying to obtain the finished etimicin sulfate.

Description

technical field [0001] The invention relates to the field of medicinal chemistry, in particular to a microwave preparation method of aminoglycoside antibiotic drug etimicin sulfate. Background technique [0002] Etimicin sulfate (Etimicin sulfate) is a new generation of semi-prepared aminoglycoside antibiotics with high efficiency, low toxicity and resistance to drug-resistant bacteria with independent intellectual property rights. It is the only one that has obtained the national first-class new drug certificate. Anti-infective drugs. It was developed by the "Jiangsu Provincial Institute of Microbiology" and has obtained patents in China, the United States, the United Kingdom, Japan, Russia, Kazakhstan and other countries, and has been widely used because of its advantages as a new type of antibacterial drug with high efficiency and low toxicity. Its mechanism of action is to resist the normal protein production of sensitive bacteria, including Escherichia coli, Klebsiella...

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Problems solved by technology

[0004] Chinese patent 201310082864.8 discloses the improvement of the preparation process of etimicin sulfate: the benzyl group is used to protect the amino group, and then hydrogen and Pd / C are used to reduce the benzyl group. The deprotection reaction of the benzyl group is completed at the same time. Although the steps are shortened, the process The hydroxyl group is not effectively protected, which is not conducive to the reduction of by-products

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