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A kind of synthetic method of etimicin sulfate

A technology of etimicin sulfate and synthesis method, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve problems such as low yield, achieve high yield, improve yield, and reduce steps Effect

Active Publication Date: 2015-12-02
福安药业集团烟台只楚药业有限公司
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Problems solved by technology

This existing etimicin sulfate synthetic method technological yield is 36%, and yield is low

Method used

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  • A kind of synthetic method of etimicin sulfate
  • A kind of synthetic method of etimicin sulfate
  • A kind of synthetic method of etimicin sulfate

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Embodiment Construction

[0036] The present invention is the preparation method of synthesizing etimicin by gentamicin C1a, specifically comprises the following steps:

[0037] 1. Get 1500 grams of gentamicin C1a and add it into a stainless steel reaction tank with interlayer heating and stirring functions with a volume of 50 liters, then add 30 liters of methanol in the reaction tank (according to 1 gram of gentamicin C1a, add methanol 20 ml), stirred for 30 minutes at a stirring speed of 80 rpm, so that gentamicin C1a was fully mixed into methanol to obtain a methanol solution of gentamicin C1a.

[0038] Gentamicin C1a is one of the components of gentamicin, which is white or off-white powder, easily soluble in water, slightly soluble in methanol, acetone and other organic solvents, the chemical structural formula of gentamicin C1a:

[0039]

[0040] Molecular weight of Gentamicin C1a: 449

[0041] Molecular formula of gentamicin C1a: C 19 h 39 N 5 o 7

[0042] 2. Add 2000 grams of zinc ace...

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Abstract

The invention discloses a synthetic method of etimicin sulfate. The synthetic method comprises the following steps: carrying out a reaction on gentamicin C1a, zinc acetate and acetic anhydride to obtain 3, 2', 6'-tri(N-acetyl) gentamicin C1a; after separating and purifying the 3, 2', 6-tri(N-acetyl) gentamicin C1a, carrying out a reaction with iodoethane to obtain 3, 2', 6'-tri(N-acetyl)-1-ethyl gentamicin C1a; hydrolyzing the 3, 2', 6'-tri(N-acetyl)-1-ethyl gentamicin C1a by sodium hydroxide to obtain an aqueous solution of etimicin sulfate; and carrying out HZD-2 macroporous resin adsorption, separation and purification, concentration, sulfate formation, decarburization and drying on the aqueous solution of etimicin sulfate to obtain an etimicin sulfate finished product. The method disclosed by the invention is high in yield which is 55%, and satisfies the requirements of Chinese pharmacopoeia (Edition 2010).

Description

technical field [0001] The invention relates to a preparation method of etimicin sulfate, in particular to a preparation method for synthesizing etimicin sulfate from gentamicin C1a, and belongs to the technical field of semi-synthesis of aminoglycoside drugs. Background technique [0002] Etimicin sulfate is a new semi-synthetic water-soluble aminoglycoside antibiotic, and its mechanism of action is to inhibit the normal protein synthesis of sensitive bacteria. Etimicin sulfate is a broad-spectrum antibiotic, which has good antibacterial effect on most Gram-positive bacteria and negative bacteria, especially Escherichia coli, Klebsiella pneumoniae, Serratia, Salmonella and Staphylococcus. It has good antibacterial activity, and has antibacterial activity against some Staphylococcus aureus, Escherichia coli, and Klebsiella pneumoniae resistant to gentamicin, micronomycin and cefazolin, and has antibacterial activity against some Staphylococci producing penicillinase And som...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/236C07H1/00C07H1/06
Inventor 葛祥斌杨俊法孙永国王玉红张文浩李贤坤王永盛张健马金凤
Owner 福安药业集团烟台只楚药业有限公司
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