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A kind of refining method of 7-aminodesacetoxy cephalosporanic acid

The technology of an acetoxy cephalosporanic acid and a refining method, which is applied in the refining field of 7-aminodeacetoxy cephalosporanic acid, can solve the problem of high impurity content, reduce toxic and side effects, improve market competitiveness, and reduce the water content of impurities Effect

Active Publication Date: 2021-05-04
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problems that the existing 7-ADCA products have high impurity content and product quality needs to be further improved, the invention provides a method for refining 7-aminodesacetoxycephalosporanic acid

Method used

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  • A kind of refining method of 7-aminodesacetoxy cephalosporanic acid
  • A kind of refining method of 7-aminodesacetoxy cephalosporanic acid
  • A kind of refining method of 7-aminodesacetoxy cephalosporanic acid

Examples

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Embodiment 1

[0040] A method for refining 7-aminodesacetoxycephalosporanic acid:

[0041] Step 1. Weigh 5g of fully dried 7-ADCA crude product and 85mL of water into the crystallizer, control the temperature at 20°C, add 5% dilute ammonia solution with a mass fraction of 0.48mL / min to adjust the pH =8, obtain alkali solution;

[0042] Step 2, adding a sulfuric acid solution with a mass fraction of 20% to the alkali solution to adjust the pH to 0.8 to obtain an acid solution;

[0043] Step 3, adding ammonia water with a mass fraction of 13% to the acid solution, adjusting the pH to 7.8, adding 35 mL of anhydrous methanol to obtain a crystallization solution;

[0044] Step 4, at a temperature of 60°C and a stirring rate of 230r / min, add sulfuric acid with a mass fraction of 20% to the liquid to be crystallized at a dropping rate of 0.75mL / min, adjust the pH to 3.8, and grow crystals After 20 minutes, filter, wash the filter cake with water and acetone, and dry in a constant temperature dry...

Embodiment 2

[0049] A method for refining 7-aminodesacetoxycephalosporanic acid:

[0050] Step 1. Weigh 5g of fully dried 7-ADCA crude product and 95mL of water into the crystallizer, control the temperature at 25°C, add a 4% dilute ammonia solution with a mass fraction of 0.45mL / min to adjust the pH =7.8, obtain alkali solution;

[0051] Step 2, adding a sulfuric acid solution with a mass fraction of 18% to the alkali solution to adjust the pH to 0.7 to obtain an acid solution;

[0052] Step 3, adding ammonia water with a mass fraction of 15% to the acid solution, adjusting the pH to 7.9, adding 40 mL of anhydrous methanol to obtain a crystallization solution;

[0053] Step 4, at a temperature of 65°C and a stirring rate of 200r / min, add sulfuric acid with a mass fraction of 18% to the liquid to be crystallized at a dropping rate of 0.85mL / min, adjust the pH to 3.9, and grow crystals After 25 minutes, filter, wash the filter cake with water and acetone, and dry in a constant temperature...

Embodiment 3

[0056] A method for refining 7-aminodesacetoxycephalosporanic acid:

[0057] Step 1. Weigh 5g of fully dried 7-ADCA crude product and 90mL of water into the crystallizer, control the temperature at 23°C, add 3% dilute ammonia solution with a mass fraction of 0.5mL / min to adjust the pH =7.9, obtain alkali solution;

[0058] Step 2, adding a sulfuric acid solution with a mass fraction of 19% to the alkali solution to adjust the pH to 0.9 to obtain an acid solution;

[0059] Step 3, adding ammonia water with a mass fraction of 14% to the acid solution, adjusting the pH to 8.0, adding 45mL of absolute ethanol to obtain a crystallization solution;

[0060] Step 4: At a temperature of 62°C and a stirring rate of 250r / min, add sulfuric acid with a mass fraction of 20% to the liquid to be crystallized at a dropping rate of 1.0mL / min, grow crystals for 23min, filter, and water Wash the filter cake with acetone, and dry it in a constant temperature drying oven for 2 hours to obtain th...

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Abstract

The invention provides a method for refining 7-aminodesacetoxycephalosporanic acid, comprising the following steps: adding crude 7-aminodesacetoxycephalosporanic acid into water, dispersing evenly, adding ammonia water to adjust the pH to 7.8-8.0, Obtain an alkali solution; add sulfuric acid to the alkali solution to adjust the pH to 0.7-0.9 to obtain an acid solution; add ammonia to the acid solution to adjust the pH to 7.8-8.0, add alcohol to obtain a crystallization solution ; Add sulfuric acid to the liquid to be crystallized under stirring at a temperature of 20-70°C, adjust the pH to 3.8-4.0, grow the crystals for 6-60 minutes, and obtain the 7-aminodesacetoxycephalosporanic acid product. According to the refining method provided by the invention, the purity of the prepared 7-ADCA can reach more than 99.91%, the yield can reach more than 87%, and the content of Δ-2-7-ADCA is less than 0.06%, which has broad application prospects.

Description

technical field [0001] The invention relates to the technical field of pharmaceutical and chemical production, in particular to a method for refining 7-aminodesacetoxycephalosporanic acid. Background technique [0002] Cephalosporin antibiotics are widely used in the treatment of bacterial infections due to their broad spectrum and low toxicity. 7-aminodesacetoxycephalosporanic acid (7-ADCA) is an important intermediate of semi-synthetic cephalosporin antibiotics and a bridge for converting penicillin products into cephalosporin products, and its demand is gradually increasing. During the synthesis of 7-ADCA, it is easy to produce Δ-2-7-ADCA isomers in the ring expansion step or enzyme cleavage process. The structural formulas of 7-ADCA and its Δ-2-7-ADCA impurities are as follows. [0003] [0004] Use the 7-ADCA product that contains this isomer impurity, and when it is used as starting material synthetic various cephalosporins, will obviously influence the quality of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/12C07D501/18
CPCC07D501/12C07D501/18
Inventor 孙华李颖刘宝树张军立
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY