A kind of method for preparing 7-aminocephalosporanic acid

A technology for amino cephalosporanic acid and amino acid, which is applied in the field of preparing 7-amino cephalosporanic acid, can solve the problems of many impurities, many residual solvents, poor stability, etc., and achieves the reduction of the total amount of COD, the reduction of environmental requirements, and the few reaction steps. Effect

Inactive Publication Date: 2011-12-21
FUJIAN FUKANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

E. There are many impurities in the 7-aminocephalosporanic acid crystallization liquid, which can easily have an adverse effect on its crystallization process, resulting in poor crystal form, low content, high color grade, poor stability and many residual solvents
On the other hand, due to the relatively active β-lactam ring and free primary amino groups in the 7-aminocephalosporanic acid molecule, the stability is relatively poor

Method used

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  • A kind of method for preparing 7-aminocephalosporanic acid
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  • A kind of method for preparing 7-aminocephalosporanic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Add cephalosporin C sodium salt solution into the enzyme reactor, then add D-amino acid oxidase to oxidize, after hydrogen peroxide transfer, add GL-7 aminocephalosporanic acid acylase to cleavage, then crystallize, centrifugally filter, wash, Drying and testing yields 7-aminocephalosporanic acid with a purity of over 96%.

[0026] The concentration of the cephalosporin C sodium salt solution is 4%, and its preparation steps: take 48 grams of cephalosporin C sodium salt in a 1200ml beaker, add an appropriate amount of distilled water, after fully dissolving, adjust the pH to 7.0 with 3N ammonia water Left and right, remove the insoluble matter by vacuum filtration, add distilled water to 1200ml, and set aside in a constant temperature water bath at 20°C.

[0027] The input amount of the oxidase is 2500u oxidase per liter of cephalosporin C sodium salt solution.

[0028] The input amount of the acylase is 5000 u of the acylase per liter of cephalosporin C sodium salt so...

Embodiment 2

[0034] Add cephalosporin C sodium salt solution into the enzyme reactor, then add D-amino acid oxidase to oxidize, after hydrogen peroxide transfer, add GL-7 aminocephalosporanic acid acylase to cleavage, then crystallize, centrifugally filter, wash, Drying and testing yields 7-aminocephalosporanic acid with a purity of over 96%.

[0035] The concentration of the cephalosporin C sodium salt solution is 4%, and its preparation steps: take 48 grams of cephalosporin C sodium salt in a 1200ml beaker, add an appropriate amount of distilled water, after fully dissolving, adjust the pH to 7.0 with 3N ammonia water Left and right, remove the insoluble matter by vacuum filtration, add distilled water to 1200ml, and set aside in a constant temperature water bath at 20°C.

[0036] The input amount of the oxidase is 2500u oxidase per liter of cephalosporin C sodium salt solution.

[0037] The input amount of the acylase is 5000 u of the acylase per liter of cephalosporin C sodium salt so...

Embodiment 3

[0043] 7-Aminocephalosporanic acid double enzyme conversion HPLC analysis method

[0044] 1. Preparation of mobile phase

[0045] 1. Phase A

[0046] Weigh 1.542g of ammonium acetate and add 1000ml of distilled water to dissolve it, adjust the pH to 4.5 with glacial acetic acid, filter through a 0.45μm water filter and degas for 20 minutes.

[0047] 2. Phase B

[0048] Measure 900ml of phase A, add 100ml of acetonitrile and mix well, then degas for 20min.

[0049] 2. HPLC analysis conditions

[0050] Column type: Rp-8e, 5μm, LiChroCART 250-4

[0051] Total flow rate: 1.0ml / min

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Abstract

The invention is a method for preparing 7-aminocephalosporanic acid. Add cephalosporin C sodium salt solution in the enzyme reactor, then add D-amino acid oxidase to oxidize, after hydrogen peroxide conversion, add GL-7 aminocephalosporanic acid acylase to cleavage, then crystallize, centrifugal filter, wash, Dry and test to get 7-aminocephalosporanic acid. The production process is greatly simplified. The cephalosporin C obtained by fermentation can be used for enzymolysis without crystallization. No toxic solvent is used in the production process, and steps such as adding and removing protective agents are omitted. The product can achieve high yield and high yield. quality while reducing costs and pollution.

Description

technical field [0001] The invention relates to the field of drug synthesis, in particular to a method for preparing 7-aminocephalosporanic acid by adopting a microbial method. Background technique [0002] 7-Aminocephalosporanic acid, with a molecular weight of 272.27, is a key intermediate of cephalosporin (β-lactam) antibiotics. The production process is to prepare Cephalosporin C through biological fermentation and chemical extraction, and then chemically crack or enzymatically decompose Cephalosporin C into 7-aminocephalosporanic acid. 7-Aminocephalosporanic acid has two active groups, the acetoxy group at the 3-position and the amino group at the 7-position. Different side chains are connected to these two active groups to form cephalosporin antibiotics with different properties. It can produce more than 80 kinds of downstream cephalosporin antibiotic products, such as cefotaxime sodium, ceftriaxone sodium, cefmetazole sodium, cefuroxime sodium, cefoperazone sodium, ...

Claims

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Application Information

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IPC IPC(8): C12P35/02
Inventor 赵松
Owner FUJIAN FUKANG PHARMA
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