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Method for preparing ceftazidime pentahydrate

A technology for ceftazidime and pentahydrate, which is applied in the field of preparation of ceftazidime pentahydrate, can solve the problems of high content of impurities and polymers, complicated operation, poor crystal form and the like, and achieves the effects of high yield, simple operation and high purity

Inactive Publication Date: 2009-12-23
SHANGHAI NEW ASIA PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The technical problem to be solved by the present invention is to provide a method for preparing ceftazidime pentahydrate with low cost, safe and convenient operation, high purity, high yield and reduced pollution, so as to overcome the high cost and cumbersome operation caused by adding acid solution problems, as well as the problems of low purity of direct crystallization, high content of impurities and polymers, and poor crystal form

Method used

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  • Method for preparing ceftazidime pentahydrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A preparation method of ceftazidime pentahydrate, carried out according to the following steps:

[0029] Step 1. Inject 30ml of water for injection into the dissolving tank, add 18g of ceftazidime hydrochloride, after dissolving, put in 0.5g of activated carbon, decolorize for 30 minutes, filter, and the filtrate is set aside;

[0030] Step 2, inject 45ml of water for injection into another dissolving tank, add 25g of ceftazidime hydrochloride, after dissolving, put in 0.5g of activated carbon, decolorize for 30 minutes, filter, and transfer the filtrate to a crystallization tank;

[0031] Step 3. Add dropwise the equivalent concentration of 3N sodium hydroxide solution to the crystallization tank in the second step, adjust the pH to 4.8, then add the filtrate in the first step dropwise to adjust the pH value to 3.6, and keep the temperature at 0-10°C , stirred, crystallized;

[0032] Step 4: After growing the crystal for 3-4 hours, filter, wash the filter cake twice w...

Embodiment 2

[0035] A preparation method of ceftazidime pentahydrate, carried out according to the following steps:

[0036] Step 1. Inject 60ml of water for injection into the dissolving tank, add 37g of ceftazidime hydrochloride, after dissolving, put in 1.5g of activated carbon, decolorize for 30 minutes, filter, and the filtrate is set aside;

[0037] Step 2, inject 100ml of water for injection into another dissolving tank, add 54g of ceftazidime hydrochloride, after dissolving, put in 1.5g of activated carbon, decolorize for 30 minutes, filter, and transfer the filtrate to a crystallization tank;

[0038] Step 3. Add 20% sodium carbonate solution dropwise to the crystallization tank in the second step, adjust the pH value to 5.0, then add the filtrate in the first step dropwise to bring the pH value back to 3.6, keep the temperature at 0-10°C, and stir ,crystallization;

[0039] Step 4: After growing the crystal for 3-4 hours, filter, wash the filter cake twice with cold water and ac...

Embodiment 3

[0042] A preparation method of ceftazidime pentahydrate, carried out according to the following steps:

[0043] Step 1. Inject 50ml of water for injection into the dissolving tank, add 32g of ceftazidime hydrochloride, after dissolving, put in 1.5g of activated carbon, decolorize for 30 minutes, filter, and the filtrate is set aside;

[0044] Step 2, inject 80ml of water for injection into another dissolution tank, add 48g of ceftazime hydrochloride, after dissolving, put in 1.5g of activated carbon, decolorize for 30 minutes, filter, and transfer the filtrate to a crystallization tank;

[0045] Step 3, add 8% sodium bicarbonate solution dropwise to the crystallization tank in the second step, adjust the pH value to 5.3, then add the filtrate in the first step dropwise to bring the pH value back to 3.6, and keep the temperature at 0-10°C, stir, crystallize;

[0046] Step 4: After growing the crystal for 3-4 hours, filter, wash the filter cake twice with cold water and acetone...

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Abstract

The invention discloses a method for preparing ceftazidime pentahydrate, which comprises the following steps: 1, filling water for injection in a dissolving tank, adding a ceftazidime hydrochloride into the dissolving tank, putting active carbon into the dissolving tank for decolorization after the ceftazidime hydrochloride is dissolved and filtering the solution to obtain filtrate for later use; 2, filling water for injection in another dissolving tank, adding the ceftazidime hydrochloride into the dissolving tank, putting active carbon into the dissolving tank for decolorization after the ceftazidime hydrochloride is dissolved, filtering the solution and transferring filtrate into a crystallizing tank; 3, dripping alkaline solution into the crystallizing tank in the step 2 to adjust the pH value of the filtrate to 4.0 to 6.0, dripping the filtrate obtained by the step 1 into the crystallizing tank to adjust the pH value of the filtrate back to 3.6, keeping the temperature at 0 to 10 DEG C and stirring the mixed solution for crystallization; and 4, growing crystals for 3 to 4 hours, filtering the mixed solution, washing a filter cake with cold water and acetone respectively and drying the filter cake under vacuum for 2 to 3 hours to obtain the ceftazidime pentahydrate. The method has the advantages of saving capital, simplifying process, reducing discharged waste gas and water, along with simple and convenient operation, suitability for industrial production, high purity and high yield.

Description

technical field [0001] The invention relates to a preparation method of ceftazidime pentahydrate. Background technique [0002] Ceftazime pentahydrate, the chemical name is (6R,7R)-7-[[(2-amino-4-thiazolyl)-[(1-carboxy-1-methylethoxy)imino]acetyl]amino ]-2-Carboxy-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-3-methylpyridinium inner salt pentahydrate. The structural formula is as follows: [0003] [0004] Ceftazidime is a third-generation cephalosporin antibiotic. It is used for the treatment of sepsis, lower respiratory tract infection, abdominal cavity and biliary tract infection, complicated urinary tract infection and severe skin and soft tissue infection caused by sensitive Gram-negative bacilli. It is especially suitable for infection of immunocompromised persons caused by multiple drug-resistant Gram-negative bacilli, nosocomial infections, and central nervous system infections caused by Gram-negative bacilli or Pseudomonas aeruginosa. Because ceftazidime pentahy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/46A61P31/04
Inventor 郑玉林管海英李晴
Owner SHANGHAI NEW ASIA PHARMA
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