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A kind of synthetic method of aminoglycoside compound

A technology of aminoglycosides and synthesis methods, which is applied in the field of organic chemical synthesis, can solve the problems of no synthesis and separation methods, acquisition, and purchase, and achieve less toxic reagents and solvents, high environmental friendliness, and less waste water discharge Effect

Active Publication Date: 2021-11-16
WUXI JIYU SHANHE PHARM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, this compound cannot be purchased directly from the market, and there is no easy synthesis and separation method to obtain it.

Method used

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  • A kind of synthetic method of aminoglycoside compound
  • A kind of synthetic method of aminoglycoside compound
  • A kind of synthetic method of aminoglycoside compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Dissolve commercially available etimicin sulfate in water at a mass volume ratio of 1:13, and add nitrous acid at a ratio of 1:1; adjust the pH to 1 with 1 mol / L dilute sulfuric acid at -5°C , kept stirring for 1 hour to obtain a reaction solution; the reaction solution was added with stannous chloride according to the ratio of the amount of etimicin sulfate substance 1:1, and reacted at 10°C for 2 hours to obtain a reaction product; the reactant was adsorbed with D1300 macropores Resin adsorption, then elute with 10% ethanol by volume, detect the components of the eluent by TLC method, and collect the eluent whose target components meet the requirements; the eluent is vacuum-raised and concentrated to a concentrated solution with a dry matter content of 25% , freeze-dried to obtain the target product.

Embodiment 2

[0054] Dissolve commercially available etimicin sulfate in water at a mass volume ratio of 1:14, and add sodium nitrite at a ratio of 1:1.1; adjust the pH to 2 with 2 mol / L dilute sulfuric acid at 0°C , heat preservation and stirring for 2 hours to obtain a reaction solution; the reaction solution was added with aluminum powder according to the ratio of the amount of etimicin sulfate substance 1:2, and reacted at 30°C for 0.5 hours to obtain a reaction product; the reaction product was used for Huazhen chromatography No. 1 Macroporous adsorption resin adsorption, and then elute with 15% ethanol by volume percentage, detect the components of the eluent by TLC method, collect the eluent whose target component meets the requirements; The concentrated solution was vacuum-dried to obtain the target product.

Embodiment 3

[0056] Take commercially available etimicin sulfate and dissolve it in water at a mass volume ratio of 1:15, add nitrous acid at a mass-volume ratio of 1:1.5; adjust the pH to 1.5 with 1.5 mol / L dilute sulfuric acid at 5°C , insulated and stirred for 1.5 hours to obtain a reaction solution; the reaction solution was added with stannous chloride according to the ratio of the amount of etimicin sulfate substance 1:1.5, and reacted at 35°C for 1.5 hours to obtain a reaction product; the reactant was adsorbed with D101 macropores Resin adsorption, then elute with 18% ethanol by volume, detect the components of the eluent by TLC method, collect the eluent whose target component meets the requirements; wash the concentrated solution with a vacuum rising film concentration to a dry matter content of 28%, and freeze Dry to obtain the target product.

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PUM

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Abstract

The present invention relates to a synthesis method of aminoglycoside compounds. The method comprises the following steps: 1) taking etimicin sulfate and dissolving it in a solvent, adding reaction reagent A; adjusting the pH to acidity with acid, and obtaining Reaction solution; 2) Reagent B is added to the reaction solution, and the reactant is obtained after the reaction is completed; 3) The reactant is adsorbed with a macroporous adsorption resin, eluted with ethanol, and the eluent of the target component is collected; the eluent is concentrated and dried to obtain product. The structure of the aminoglycoside compound is as follows:

Description

technical field [0001] The present invention relates to an organic chemical synthesis method, specifically a 0-2-amino-2,3,4,6-tetradeoxy-6-hydroxyl-α-D-erythro-hexyranosyl- (1→4)-0-[3-deoxy-4-C-methyl-3(methylamino)-β-L-arabinopyranosyl-(1→6)]-2-deoxy-N-ethyl Synthetic method of base-L-streptomycin. Background technique [0002] Etimicin sulfate is a new generation of semi-synthetic aminoglycoside antibiotics with high efficiency, low toxicity and resistance to drug-resistant bacteria. It is the only new class of antibiotics with independent intellectual property rights in my country. Today, as the drug resistance of pathogenic bacteria is becoming more and more serious, etimicin sulfate has important clinical use value. Impurity residues in antibiotics are an important factor affecting clinical treatment effects and leading to adverse reactions in clinical use, so the research and control of impurity residues in antibiotics is of great significance. [0003] The active ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H5/06C07H1/00
CPCC07H1/00C07H5/06
Inventor 吴凌云王晓霞华梦丹
Owner WUXI JIYU SHANHE PHARM CO LTD