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Preparation method of D-7ACA

A technology of D-7ACA and 7-ACA, which is applied in the field of medicine and biology, can solve the problem that synthetic cephalosporin antibiotics are not widely used, and achieve the effects of environmental friendliness, mild reaction conditions and less side effects

Inactive Publication Date: 2018-04-20
YILI CHUANNING BIOTECH CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] D-7ACA has been discovered for nearly half a century, but it is not widely used as the parent of synthetic cephalosporin antibiotics

Method used

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  • Preparation method of D-7ACA
  • Preparation method of D-7ACA
  • Preparation method of D-7ACA

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] (1) 7-ACA dissolved

[0058] Take 5 grams of 7-ACA crystals, add them to 400ml of pure water, cool down to 6°C, and dissolve them with 5% ammonia solution by weight, and control the pH=7.8-8.0. After completely dissolving and clarifying, filter the solution with a 0.45 μm filter membrane Filtration was performed to obtain a solution of 7-ACA.

[0059] (2) Hydrolysis of 7-ACA

[0060] Stir the aforementioned solution and heat it up to 15°C, add 8 grams of deacetylesterase to the solution, use the deacetylase to hydrolyze the 3-position side chain of 7-ACA, and control the pH of the reaction with a 5% ammonia solution by weight to 8.2-8.4, use a hot water bath to control the reaction temperature to 15°C, after the reaction is complete, filter with 10 μm filter paper to obtain a hydrolyzate. Deacetylesterase was kept for future use.

[0061] (3) Primary crystallization of D-7ACA

[0062] Add dropwise hydrochloric acid with a concentration of 10% by weight to the hydrol...

Embodiment 2

[0073] (1) 7-ACA dissolved

[0074] Take 5 grams of 7-ACA crystals, add them to 500ml of pure water, cool down to 10°C, and dissolve them with an ammonia solution with a concentration of 7% by weight, and control the pH=8.2-8.4. After completely dissolving and clarifying, filter the solution with a 0.45 μm filter membrane Filtration was performed to obtain a solution of 7-ACA.

[0075] (2) Hydrolysis of 7-ACA

[0076] Stir the aforementioned solution to heat up to 18°C, add 10 grams of deacetylesterase to the solution, use the deacetylase to hydrolyze the 3-position side chain of 7-ACA, and use a 3% ammonia solution by weight to control the pH of the reaction to 8.4-8.5, use a hot water bath to control the reaction temperature to 18°C, after the reaction is complete, filter with 10 μm filter paper to obtain a hydrolyzate. Deacetylesterase was kept for future use.

[0077] (3) Primary crystallization of D-7ACA

[0078] Add dropwise hydrochloric acid with a concentration of ...

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Abstract

The invention discloses a preparation method of D-7ACA, in particular discloses a method for preparing high-purity D-7ACA and belongs to the technical field of medical biology. The method comprises the following steps: (1) dissolving 7-ACA: adding 7-ACA and ammonia water into water sequentially and filtering after completely dissolving to obtain 7-ACA solving liquid; (2) hydrolyzing the 7-ACA: adding esterase and ammonia water into the 7-ACA solving liquid sequentially and filtering after reacting completely to obtain hydrolysate; (3) crystallizing D-7ACA for the first time: adding hydrochloric acid into the hydrolysate, growing the crystal after complete crystallization and performing suction filtration to obtain a D-7ACA wet crystal; (4) dissolving the D-7ACA for the second time: sequentially adding the wet crystal and ammonia water into water sequentially, adding a resin column after completely dissolving, adsorbing and filtering to obtain a D-7ACA solution; and (5) crystallizing the D-7ACA for the second time and drying: adding hydrochloric acid into the D-7ACA solution, growing the crystal after complete crystallization, performing suction filtration, washing the crystal and drying to obtain the D-7ACA. An organic solvent is not used in the whole reaction process, the reaction condition is mild, the reaction is easy to control, the side reaction is few, and the purity of the finally prepared D-7ACA is up to 99.25 percent.

Description

technical field [0001] The invention belongs to the technical field of medicine and biology, and relates to a preparation method of D-7ACA, in particular to a method for preparing D-7ACA with relatively high purity. Background technique [0002] In the antibiotic family, cephalosporin antibiotics are a relatively large branch, and they are also commonly used clinically for the treatment of bacterial infections. The source of cephalosporin antibiotics mainly relies on synthesis or semi-synthesis, generally with 7-ACA as the parent. D-7ACA is obtained by removing the acetyl group on the 3-position of 7-ACA. The chemical name of D-7ACA is: 3-deacetyl-7-amino-cephalosporanic acid, referred to as D-7ACA, and its structural formula is : [0003] [0004] D-7ACA has been discovered for nearly half a century, but it is not widely used as the parent of synthetic cephalosporin antibiotics. With the development of bio-fermentation technology, the production cost of D-7ACA has dro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/18C07D501/12C07D501/04
CPCC07D501/04C07D501/12C07D501/18
Inventor 蔡黎明臧静努尔买买提·库达巴尔地张亚勇包蕾王喜春赵鑫张云辉胡晓非王洋
Owner YILI CHUANNING BIOTECH CO