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Method for refining cefotiam hexetil hydrochloride

A technology of cefotiam and its refining method, which is applied in the field of medicine, can solve problems such as difficulty in filtering, small product particle size, and affecting product quality, and achieve the effects of simple and easy post-processing, high product quality, and improved product yield

Active Publication Date: 2014-03-19
YIYUAN XINQUAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, in the process of producing cefotiam axetil hydrochloride, crystals coalesce, resulting in a small particle size of the final product, which is difficult to filter, and a large amount of crystallization mother liquor is mixed in the product, which affects the quality of the product

Method used

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  • Method for refining cefotiam hexetil hydrochloride
  • Method for refining cefotiam hexetil hydrochloride
  • Method for refining cefotiam hexetil hydrochloride

Examples

Experimental program
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Effect test

Embodiment 1

[0033] (1) In a three-neck flask, dissolve 1.5 mol of sodium carbonate in 600 mL of distilled water, then add 1 mol of cefotiam hydrochloride, stir at room temperature, and react for 1 hour to obtain cefotiam sodium salt.

[0034] (2) Add 1 mol of the cefotiam sodium salt obtained above and 1.5 mol of 1-iodoethyl cyclohexyl carbonate to 400 mL of dimethylformamide solvent, the reaction temperature is 10 ° C, the reaction time is 12 min, and water is added under stirring cool down.

[0035] (3) 1000 ml of ethyl acetate was added to the obtained reaction solution for extraction.

[0036] (4) Transfer the organic phase extracted in step (3) to a 5000ml three-neck bottle, place it in an ultrasonic generator, control the temperature at 15°C, and add 5 parts by volume of a mixed solvent under stirring (the mixed solvent is a mass fraction of 3% HCl and 97% acetone), after dropping, turn on ultrasonic seeding for 40min, the ultrasonic frequency is 60KHz, and then stir for 25min, the...

Embodiment 2

[0038] (1) In a three-neck flask, dissolve 2 mol of sodium bicarbonate in 700 mL of distilled water, then add 1 mol of cefotiam hydrochloride, stir at room temperature, and react for 0.5 h to obtain cefotiam sodium salt.

[0039] (2) Add 1 mol of the cefotiam sodium salt obtained above and 2 mol of 1-iodoethyl cyclohexyl carbonate to 600 mL of dimethylformamide solvent, the reaction temperature is 15 °C, the reaction time is 10 min, and cooled with water under stirring .

[0040] (3) Add 1500ml of methanol to the obtained reaction solution for extraction.

[0041] (4) Transfer the organic phase extracted in step (3) to a 5000ml three-neck bottle, place it in an ultrasonic generator, control the temperature at 10°C, and add 4 parts by volume of a mixed solvent under stirring (the mixed solvent is a mass fraction of 0.5% HCl and 99.5% acetone), after dripping, turn on the ultrasonic generator for seeding for 50min, the ultrasonic frequency is 20KHz, and then stir for 20min, the...

Embodiment 3

[0043] (1) In a three-neck flask, dissolve 1.8 mol of sodium isooctanoate in 700 mL of distilled water, then add 1 mol of cefotiam hydrochloride, stir at room temperature, and react for 0.8 h to obtain cefotiam sodium salt.

[0044] (2) Add 1 mol of the cefotiam sodium salt obtained above and 1.2 mol of 1-iodoethyl cyclohexyl carbonate to 500 mL of dimethylformamide solvent, the reaction temperature is -9 ° C, the reaction time is 20 min, under stirring Cool with water.

[0045] (3) Add 1200ml of dichloromethane to the obtained reaction solution for extraction.

[0046](4) Transfer the organic phase extracted in step (3) to a 5000ml three-neck bottle, place it in an ultrasonic generator, control the temperature at 25°C, and add 3 parts by volume of a mixed solvent under stirring (the mass fraction of the mixed solvent is 4% HCl and 96% methanol), after dripping, turn on the ultrasonic generator to seed the crystal for 30min, the ultrasonic frequency is 80KHz, then stir for 35...

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Abstract

The invention belongs to the field of medicines, and in particular relates to a method for refining cefotiam hexetil hydrochloride. The method comprises the steps: preparing cefotiam salt into cefotiam sodium salt; performing esterification reaction on a dimethylformamide solution of the cefotiam sodium salt and carbonic acid 1-iodine ethyl ester cyclohexyl acetate; adding obtained reaction liquid into an extracting agent for extracting; adding an organic phase obtained by extracting into an organic solvent for crystallizing, and crystallizing under an ultrasonic wave condition; and finally filtering to obtain cefotiam hexetil hydrochloride. Sound wave irradiation of the ultrasonic waves has a strong orientation effect and has an effect of intensifying to form the wave action required by critical crystal nucleus so as to accelerate the graining process and quickly generate the crystal nucleus; meanwhile, the coalescence condition during growth of the crystals can be avoided, and the grain distribution of the crystals is relatively uniform. The method is safe and reliable, the granularity of the obtained final product is large, the cefotiam hexetil hydrochloride product is easy to filter and high in quality; the post-treatment is easy and simple, and the quality and the yield of the product can be improved well.

Description

technical field [0001] The invention belongs to the field of medicine, and in particular relates to a method for refining cefotiam hydrochloride. Background technique [0002] Cefotiam (structural formula I), English name: Cefotiam Hexetil, English aliases: Pansporin, CTM-HE. It itself is unstable, so the medicinal form is cefotiam hydrochloride (structural formula II). Cefotiam (CTM) (structural formula III) is absorbed. . The antibacterial activity of CTM against Gram-positive and negative bacteria is the same as that of previous oral cephalosporins, and it is stable to β-lactamase. This product is effective against clinically isolated Staphylococcus aureus, coagulase-negative staphylococcus, Streptococcus pneumoniae, Neisseria gonorrhoeae, Ampicillin-resistant Neisseria gonorrhoeae (ABPC), Moraxella catarrhalis, Escherichia coli, Citric acid bacteria, Provi Denstella, Streptococcus pyogenes, Streptococcus agalactiae, Klebsiella pneumoniae, Proteus mirabilis, and Haemo...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/12
CPCC07D501/04C07D501/12C07D501/36
Inventor 刘兆花张立明
Owner YIYUAN XINQUAN CHEM
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