Method for preparing 3-deacetyl-7-aminocephalosporanic acid

A technology of aminocephalosporanic acid and deacetylation, which is applied in the field of preparation of 3-deacetyl-7-aminocephalosporanic acid, can solve problems such as difficulty in centrifugation, low yield, and long process route, and achieve low environmental protection costs , high product yield and short process route

Inactive Publication Date: 2010-06-09
石药集团中诺药业(石家庄)有限公司
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned existing D-7-ACA preparation method: the process route is long and must go through three crystallization processes of cephalosporin C sodium salt (or zinc salt), 7-ACA, and D-7-ACA, because the crystallization process yield loss many, resulting in a low yield, the calculation method a and b are respectively 65.2% and 67.8% from the molar yield of cephalosporin C extract to D-7-ACA, in addition, method a adopts chemical cracking, and its process consumes a lot of Cryogenics and solvents, and methylene chloride, aniline, and chlor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0028] Example 1

[0029] A preparation method of 3-deacetyl-7-aminocephalosporanic acid with short process route, high product yield, low manufacturing cost and suitable for large-scale production. The specific preparation process is:

[0030] 1. Take the cephalosporin C nanofiltration concentrated solution analyzed by sodium bicarbonate with a concentration of 83.3g / L and prepare 1L cephalosporin C solution with a concentration of 31.5g / L with no salt water, and put it into 1.5L enzyme reactor I ;

[0031] 2. Weigh 2.5KU D-amino acid oxidase, wash with no salt water, and put it into enzyme reactor I, stirring at 400rpm, using 3mol / L ammonia to control pH to 7.1~7.5, temperature 20℃, oxygen flow 0.1 vvm, tank pressure 1.0~1.2bar, after 60 minutes of reaction, transfer the reaction solution to enzyme reactor II (D-amino acid oxidase is intercepted by the screen at the bottom of the enzyme reactor);

[0032] 3. Weigh 3.0KU glutaryl-7-ACA acylase and 1.0KU cephalosporin esterase, mix t...

Example Embodiment

[0034] Example 2

[0035] A preparation method of 3-deacetyl-7-aminocephalosporanic acid with short process route, high product yield, low manufacturing cost and suitable for large-scale production. The specific preparation process is:

[0036] 1. Take the cephalosporin C nanofiltration concentrated solution analyzed by sodium acetate with a concentration of 95.1g / L and prepare 1L cephalosporin C solution with a concentration of 33.5g / L with no salt water, and put it into 1.5L enzyme reactor I;

[0037] 2. Weigh 4.0KU D-amino acid oxidase, wash with no salt water, and put it into enzyme reactor I, stirring at 400rpm, using 3mol / L ammonia to control pH to 7.1~7.6, temperature 20℃, oxygen flow 0.2 vvm, tank pressure 1.4~1.5bar, after 60 minutes of reaction, transfer the reaction solution to enzyme reactor II (D-amino acid oxidase is intercepted by the screen at the bottom of the enzyme reactor);

[0038] 3. Weigh 5.0KU glutaryl-7-ACA acylase and 2.0KU cephalosporin esterase, mix them, w...

Example Embodiment

[0040] Example 3

[0041] A preparation method of 3-deacetyl-7-aminocephalosporanic acid with short process route, high product yield, low manufacturing cost and suitable for large-scale production. The specific preparation process is:

[0042] 1. Take the cephalosporin C concentrated solution resolved by ammonium acetate with a concentration of 67.3g / L and prepare 1L cephalosporin C solution with a concentration of 40.2g / L with no salt water, and put it into 1.5L enzyme reactor I;

[0043] 2. Weigh 6.0KU D-amino acid oxidase, wash it with no salt water, and put it into enzyme reactor I, stirring at 400rpm, using 3mol / L ammonia to control pH to 7.1~7.6, temperature 20℃, oxygen flow 0.3vvm , The tank pressure is 1.4 ~ 1.5 bar, after 70 minutes of reaction, the reaction solution is transferred to the enzyme reactor II (D-amino acid oxidase is intercepted by the screen at the bottom of the enzyme reactor);

[0044] 3. Weigh 7.0KU glutaryl-7-ACA acylase and 3.5KU cephalosporin esterase, m...

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Abstract

The invention discloses a method for preparing 3-deacetyl-7-aminocephalosporanic acid, which comprises the following steps: catalyzing extract of cephalosporin C serving as a raw material by D-amino-acid oxidase to prepare solution of glutaryl-7-ACA; catalyzing the solution of glutaryl-7-ACA by glutaryl-7-ACA acylase and cephalosporin esterase to prepare solution of 3- deacetyl-7-aminocephalosporanic acid; and performing acidification crystallization, washing and drying to obtain solid 3-deacetyl-7-aminocephalosporanic acid. The method for preparing the3-deacetyl-7-aminocephalosporanic acid only needs two steps of normal temperature reaction and one-time crystallization process and has short process route; solvents are not used basically; the molar yield from the extract of the cephalosporin C to the 3-deacetyl-7-aminocephalosporanic acid can reach 71.5 percent; and the yield of the product is high. In addition, compared with the prior art, the method has much lower energy consumption, power cost, labor cost and environmental cost.

Description

technical field [0001] The invention relates to a preparation method of pharmaceutical raw materials, in particular to a preparation method of 3-deacetyl-7-aminocephalosporanic acid. Background technique [0002] 3-Deacetyl-7-aminocephalosporanic acid is referred to as D-7-ACA. Because the 7-position amino group and 3-position hydroxyl group of D-7-ACA are relatively active, different side chains can be introduced to synthesize a series of cephalosporin antibiotics according to the needs. , such as cefuroxime, cefpirome, cefcapene, cefixime, cefdinir, ceftazidime, etc. Cephalosporin antibiotics have the characteristics of broad-spectrum antibacterial properties and small toxic and side effects. They are currently the most widely used antibiotics in clinical practice. The demand for 7-ACA is also increasing. [0003] The method for preparing D-7-ACA mainly contains two kinds at present: a. Cephalosporin C sodium salt (or zinc salt) obtains 7-ACA (7-aminocephalosporin) by es...

Claims

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Application Information

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IPC IPC(8): C12P35/00
Inventor 卢华刘桂军朱科康辉辛朝辉王峰王艳艳丁海平延国东薛瀚孟德程
Owner 石药集团中诺药业(石家庄)有限公司
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