Method for crystallizing and producing cefpiramide sodium crystals

A technology of cefpiramide sodium and cefpiramic acid, which is applied in the field of medicine and chemical industry, can solve the problems of poor fluidity, difficulty in dispensing, and easy precipitation, and achieve the effects of good fluidity, easy dispensing, and good solubility

Active Publication Date: 2013-09-25
NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The transamination agents used in this patent are triethylamine, diethylamine, and ethylenediamine, which are highly toxic, and the resulting amine salts have poor solubility in their solvent systems and are easy to separate out
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  • Method for crystallizing and producing cefpiramide sodium crystals

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039]Accurately measure 20g of cefpiramin, 60ml of methanol, 40ml of acetone, 20ml of acetonitrile, and 4.6ml of triethylamine into a four-necked bottle. The molar ratio of cefpiramin and triethylamine is 1:1. The ratio of the weight in grams to the volume in milliliters of the solvent I is 1:6. In a constant temperature reaction bath at 20°C, stir until completely dissolved to form a cefpiramide salt solution for later use. Accurately measure 1.5g of sodium hydroxide and 40ml of methanol into a conical flask. The amount of sodium hydroxide added is such that the molar ratio of sodium hydroxide to cefpiramin is 1.15:1. Stir until completely dissolved to form a hydroxide Sodium solution for later use. In a constant temperature reaction bath at 20°C, the sodium hydroxide solution was evenly added to the cefpiramide salt solution within 20 minutes, and then 0.03 g of cefpiramide sodium crystals were added as seed crystals, and the crystals were grown for 10 minutes. Then add 30...

Embodiment 2

[0041] Accurately measure 20g of cefpiramin, 60ml of methanol, 40ml of acetone, 20ml of acetonitrile, and 4.6ml of diisopropylamine into a four-necked bottle. The molar ratio of cefpiramin and diisopropylamine is 1:1. The ratio of the weight in grams to the volume in milliliters of solvent I is 1:6. Stir in a constant temperature reaction bath at 10°C until it is completely dissolved to form a cefpiramide salt solution for later use. Accurately measure 5.42g of sodium isooctanoate and 150ml of acetone into a conical flask. The amount of sodium isooctanoate is to make the molar ratio of sodium isooctanoate to cefpiramide 1:1, and stir until completely dissolved to form sodium isooctanoate The solution is ready for use. In a constant temperature reaction bath at 25°C, the sodium isooctanoate solution was evenly added to the cefpiramide salt solution within 25 minutes, and then 0.02 g of cefpiramide sodium crystals were added as seed crystals, and the crystals were grown for 25 m...

Embodiment 3

[0043] Accurately measure 20g of cefpiramin, 60ml of methanol, 40ml of acetone, 10ml of water, and 4.6ml of diisopropylamine into a four-neck bottle. The molar ratio of cefpiramin and diisopropylamine is 1:1. The ratio of the weight in grams to the volume in milliliters of solvent I is 1:5.5. Stir in a constant temperature reaction bath at 20°C until it is completely dissolved to form a cefpiramide salt solution for later use. Accurately measure 5.42g of sodium isooctanoate and 150ml of acetone into a conical flask. The amount of sodium isooctanoate is to make the molar ratio of sodium isooctanoate to cefpiramide 1:1, and stir until completely dissolved to form sodium isooctanoate The solution is ready for use. In a constant temperature reaction bath at 15°C, the sodium isooctanoate solution was evenly added to the cefpiramide salt solution in 30 minutes, and then 0.04 g of cefpiramide sodium crystals were added as seed crystals, and the crystals were grown for 15 minutes. Th...

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Abstract

The invention discloses a method for crystallizing and producing cefpiramide sodium crystals. The method comprises the steps that: (a) cefpiramide acid and an transamination agent are dissolved in a solvent I, wherein the transamination agent is any one selected from triethylamine, diisopropylamine, and isopropylamine; and a temperature is controlled, and the materials are stirred until completely dissolved; (b) a salt-forming agent is added into a solvent II, wherein when the salt-forming agent is sodium ethylhexanoate, the solvent II is an acetone solvent, and when the salt-forming agent is sodium hydroxide, the solvent II is any one or a mixture of two selected from methanol and tetrahydrofuran; and the materials are stirred until completely dissolved; (c) the salt-forming agent solution is uniformly added into the solution of cefpiramide amine salt; the temperature is controlled, and crystal seeds are added; curing crystallization is carried out; acetone is added into the crystallization system for regulating the pH value of the crystallization system and for carrying out solvent-out crystallization; and filtering, washing, and drying are carried out, such that the cefpiramide sodium crystals are obtained. The method provided by the invention has the advantages of simple operation, uniform crystals, high purity, low impurity content, good stability, easy storage, and the like.

Description

technical field [0001] The invention relates to a method for producing preparations in the field of medicine and chemical industry, in particular to a method for producing cefpiramide sodium crystals by a crystallization method. Background technique [0002] The chemical name of cefpiramide sodium is (6R,7R)-7-[(R)-2-(4-hydroxy-6-methyl-3-pyridylhydroxyamino)-2-(p-hydroxyphenyl)acetamido ]-3-[[(1-methyl-1H-tetrazol-5-yl)thio]methyl]-8-oxo-5-thia-1azabicyclo[4,2,0]octane- 2-ene-2-carboxylic acid sodium salt. Molecular formula: C 25 h 23 N 8 NaO 7 S 2 , whose structural formula is: [0003] [0004] This product is a third-generation cephalosporin antibiotic, used for sepsis, pneumonia, pulmonary suppuration, and prostatitis caused by sensitive bacteria such as Staphylococcus, Peptococcus, Enterobacter, Proteus, Influenza Bacillus, and Streptococcus. , acute and chronic bronchitis, cholecystitis, intrauterine infection, etc. [0005] At present, the domestic cefpir...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/04
Inventor 魏青杰高志刚陈建军张春波李惠芬蔡秋琴胡利敏
Owner NORTH CHINA PHARMA HEBEI HUAMIN PHARMA
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