Crystallization method of cefadroxil monohydrate and crystals

A technology of cefadroxil monohydrate and cefadroxil, which is applied in the field of cefadroxil monohydrate tetragonal flaky crystals, can solve the problems of product degradation, wide particle size distribution, and decreased yield, and achieve avoidance of agglomeration and uniform particle size distribution Effect

Active Publication Date: 2013-03-13
TIANJIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because the domestic enzyme immobilization technology is not mature enough, and the reaction reagent will cause the degradation of the acylase, which will cause the loss of about 10% of the enzyme
[0010] Crystallization of cefadroxil monohydrate by known crystallization methods that have been found in the art can lead to problems such as cefadroxil agglomeration or degradation, product impurity or decreased yield, wide particle size distribution, etc.
Therefore need to invent a kind of new suitable crystallization method to promote the industrialized production of cefadroxil monohydrate, simultaneously solve the problems such as product degradation in production, productive rate decline, particle size distribution width

Method used

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  • Crystallization method of cefadroxil monohydrate and crystals
  • Crystallization method of cefadroxil monohydrate and crystals
  • Crystallization method of cefadroxil monohydrate and crystals

Examples

Experimental program
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Embodiment 1

[0037] Preparation of crystalline cefadroxil monohydrate:

[0038] 1) First, 60 g of anhydrous salt water is added to the crystallizer, and then 15 g of DMF is added thereto. Add the weighed 50g cefadroxil DMF solvent compound in its mixed solvent then, maintain feed temperature simultaneously at 25 ± 1 ℃, stir to obtain the suspension of cefadroxil DMF solvent compound, and drop ammoniacal liquor at any time to keep solution The pH value is 6.7-7.0, and the concentration of ammonia water is NH 3 The content is 5% (w / w);

[0039] 2) Determine whether the cefadroxil DMF solvent compound has been completely transformed into cefadroxil monohydrate by microscope observation or refractive index detection. Treat that the crystals have all been converted, quickly turn down the stirring speed of the cefadroxil suspension, then add hydrochloric acid to adjust the pH value of the solution, and the pH value will be reduced to 4.8-5.0 through 10 minutes, and the concentration of hydroch...

Embodiment 2

[0044] Preparation of crystalline cefadroxil monohydrate:

[0045] 1) Firstly, 200g of anhydrous salt water is added into the crystallizer, and then 20g of DMF is added thereto. Add the weighed 157g cefadroxil DMF solvent compound in its mixed solvent then, maintain feed temperature simultaneously at 25 ± 1 ℃, stir to obtain the suspension of cefadroxil DMF solvent compound, and drop ammoniacal liquor at any time to keep solution The pH value is between 6.5-6.8, and the concentration of ammonia water is NH 3 The content is 10% (w / w);

[0046] 2) Determine whether the cefadroxil DMF solvent compound has been completely transformed into cefadroxil monohydrate by microscope observation or refractive index detection. After all the crystals have been converted, slow down the stirring speed of the cefadroxil suspension, then add hydrochloric acid to adjust the pH value of the solution, and reduce the pH value to 4.8-5.0 after 15 minutes, and the concentration of hydrochloric acid ...

Embodiment 3

[0052] Preparation of crystalline cefadroxil monohydrate:

[0053] 1) First, 100 g of anhydrous salt water is added to the crystallizer, and then 20 g of DMF is added thereto. Add the weighed 75g cefadroxil DMF solvent compound in its mixed solvent then, maintain feed temperature simultaneously at 19 ± 1 ℃, stir to obtain the suspension of cefadroxil DMF solvent compound, and drop ammoniacal liquor at any time to keep solution The pH value is between 6.4-6.7, and the concentration of ammonia water is NH 3 The content is 10% (w / w);

[0054] 2) Determine whether the cefadroxil DMF solvent compound has been completely transformed into cefadroxil monohydrate by microscope observation or refractive index detection. After all the crystals have been converted, slow down the stirring speed of the cefadroxil suspension, then add hydrochloric acid to adjust the pH value of the solution, and reduce the pH value to 4.8-5.0 after 4 minutes, and the concentration of hydrochloric acid is 7...

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Abstract

The invention relates to a method for producing crystals of cefadroxil monohydrate, comprising the following steps: adding an N, N-dimethyl formamide solvent compound of cefadroxil to a mixed solvent of N, N-dimethyl formamide and water, wherein the mass ratio of the cefadroxil solvent compound to the mixed solvent is 1:1-1:2, stirring to obtain a suspending liquid, and keeping the temperature at 15-30 DGE C and the pH value of the solution at 6.0-7.5 during feeding; after the cefadroxil solvent compound is totally changed into the cefadroxil monohydrate, reducing the pH value of the suspending liquid to 4.5-5.0 within 1-20 minutes, keeping the temperature at 10-18 DEGC, and stirring for crystal cultivation for 10-90 minutes; and filtering, washing and drying after crystal cultivation is finished to obtain a product, the square platy crystal-form cefadroxil monohydrate. The square platy crystal-form cefadroxil monohydrate obtained by the method has uniform particle size distribution, does not generate coalescence, and is applicable to industrial production.

Description

technical field [0001] The present invention relates to an effective method for preparing crystalline cefadroxil monohydrate. Specifically, it is a method for indirectly obtaining cefadroxil monohydrate tetragonal flaky crystals through the crystal transformation of cefadroxil solvate compound. The tetragonal flaky cefadroxil monohydrate obtained by the method has uniform particle size distribution and no agglomeration, and is suitable for industrial production. Background technique [0002] Cefadroxil, the chemical name is 7-{[amino-(4-hydroxyphenyl)acetyl]amino}-3-methyl-8-oxo-5-thia-1-azabicyclo[4,2 , 0]-2-octene-2-hydroxy acid, which is a well-known antibiotic with antibacterial activity, is a second-generation oral cephalosporin developed by American Brestel-Meyer Company, with antibacterial spectrum Wide range, weak antigenicity, good curative effect, low toxicity and safe use. [0003] At present, the cefadroxil products on the market are generally cefadroxil monoh...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D501/12
Inventor 龚俊波侯静美刘胜张军立张美景王静康尹秋响王永莉侯宝红董伟兵
Owner TIANJIN UNIV
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