Method for preparing cefmetazole sodium

Abstract

The invention relates to a method for preparing cefmetazole sodium, comprising the following steps of: undergoing a reaction of cefmetazole acid and sodium isocaprylate, then purifying, crystallizing, filtering, washing and drying to obtain a finished product. The method for preparing the cefmetazole sodium, provided by the invention, is scientific and reasonable, simple and practicable; and the obtained product has the advantages of stable quality performance, high content, low impurity content, allergy avoidance, and the like.

Description

technical field

[0001] The invention relates to a synthesis method of western medicine, in particular to a preparation method of cefmetazole sodium. Background technique

[0002] Cefmetazole is a semi-synthetic Aspergillus cephalosporin antibiotic created by Sankyo Corporation of Japan. At present, the most commonly used method for large-scale production is the reaction of thioglycolic acid and chloroacetonitrile to generate side chains, which react with 7MAC to generate cefmetazole benzyl ester, and then deprotect to generate Cefmetazole acid.

[0003] The preparation method of cefmetazole sodium: suspending cefmetazole acid in water, adding sodium hydroxide or sodium bicarbonate to dissolve it, and then separating the sodium salt by freeze-drying or spray-drying, this method has low product content and degradation The substance content is high, and the product is prone to deficiencies such as allergies. Contents of the invention

[0004] The purpose of the invention is...

Examples

Embodiment 1

[0028] Dissolve 4.3 grams of sodium isooctanoate in 50 milliliters of anhydrous methanol, control the temperature at 10-15 ° C, add 10 grams of cefmetazole acid, stir to dissolve, add 0.5 grams of activated carbon, and filter through carbon removal and sterile filtration, and use 10 Wash with one milliliter of anhydrous methanol, combine the filtrate and lotion, control the reaction temperature at 10-15°C, add 180 milliliters of isopropyl ether dropwise in 120 minutes, continue stirring for 60 minutes, filter with suction, and wash with 60 milliliters of isopropanol three times. Finally, dry in vacuum to obtain the cefmetazole sodium product.

Embodiment 2

[0030] Dissolve 4.3 grams of sodium isooctanoate in 50 milliliters of anhydrous methanol, control the temperature at 10-15 ° C, add 10 grams of cefmetazole acid, stir to dissolve, add 0.5 grams of activated carbon, and filter through carbon removal and sterile filtration, and use 10 Wash with one milliliter of anhydrous methanol, combine the filtrate and washing solution, control the reaction temperature at 10-15°C, drop the combined solution into 180 ml of isopropyl ether, continue stirring for 60 minutes, filter with suction, and wash with 60 ml of isopropanol three times. Finally, dry in vacuum to obtain the cefmetazole sodium product.

[0031] The preparation method of the cefmetazole sodium of the present invention is scientific and reasonable, simple and easy to implement, and has the advantages of high product content and less impurities.

technical field

[0001] The invention relates to a synthesis method of western medicine, in particular to a preparation method of cefmetazole sodium. Background technique

[0002] Cefmetazole is a semi-synthetic Aspergillus cephalosporin antibiotic created by Sankyo Corporation of Japan. At present, the most commonly used method for large-scale production is the reaction of thioglycolic acid and chloroacetonitrile to generate side chains, which react with 7MAC to generate cefmetazole benzyl ester, and then deprotect to generate Cefmetazole acid.

[0003] The preparation method of cefmetazole sodium: suspending cefmetazole acid in water, adding sodium hydroxide or sodium bicarbonate to dissolve it, and then separating the sodium salt by freeze-drying or spray-drying, this method has low product content and degradation The substance content is high, and the product is prone to deficiencies such as allergies. Contents of the invention

[0004] The purpose of the invention is...

Examples

Embodiment 1

[0028] Dissolve 4.3 grams of sodium isooctanoate in 50 milliliters of anhydrous methanol, control the temperature at 10-15 ° C, add 10 grams of cefmetazole acid, stir to dissolve, add 0.5 grams of activated carbon, and filter through carbon removal and sterile filtration, and use 10 Wash with one milliliter of anhydrous methanol, combine the filtrate and lotion, control the reaction temperature at 10-15°C, add 180 milliliters of isopropyl ether dropwise in 120 minutes, continue stirring for 60 minutes, filter with suction, and wash with 60 milliliters of isopropanol three times. Finally, dry in vacuum to obtain the cefmetazole sodium product.

Embodiment 2

[0030] Dissolve 4.3 grams of sodium isooctanoate in 50 milliliters of anhydrous methanol, control the temperature at 10-15 ° C, add 10 grams of cefmetazole acid, stir to dissolve, add 0.5 grams of activated carbon, and filter through carbon removal and sterile filtration, and use 10 Wash with one milliliter of anhydrous methanol, combine the filtrate and washing solution, control the reaction temperature at 10-15°C, drop the combined solution into 180 ml of isopropyl ether, continue stirring for 60 minutes, filter with suction, and wash with 60 ml of isopropanol three times. Finally, dry in vacuum to obtain the cefmetazole sodium product.

[0031] The preparation method of the cefmetazole sodium of the present invention is scientific and reasonable, simple and easy to implement, and has the advantages of high product content and less impurities.

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