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Preparation method of 3-hydroxymethyl cefotaxime

A technology of hydroxymethyl cefotaxime and cefotaxime, which is applied in the directions of resisting vector-borne diseases, organic chemistry, fermentation, etc., can solve the problems of many steps, complicated operations, etc., and achieves mild reaction conditions, simple and easy-to-control operations, The effect of high product conversion rate

Active Publication Date: 2021-03-09
河北合佳创新医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method is complicated to operate, has many steps, and requires strict process control points.

Method used

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  • Preparation method of 3-hydroxymethyl cefotaxime
  • Preparation method of 3-hydroxymethyl cefotaxime
  • Preparation method of 3-hydroxymethyl cefotaxime

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1: In a 500 ml of four-mouth flasks, 20 g of cefosporoalic acid and 160 ml of purified water were added, and the temperature of 25 ° C to 30 ° C was added, stirred well, and the 3 mol / L ammonia solution was added to 7.0 to 7.5, stirred after 5 min. 4 g of ceftriacin C-denyloy was added, and the pH was allowed to be finely adjusted with 3 mol / L ammonia solution, and the reaction was completed when the pH was maintained for 5 minutes, then filtered, filtered, filtered, and filtered to the cefosporin C to acerase. Collect the filtrate;

[0025] When the above filtrate temperature was 10 to 15 ° C, a mixed solution of 5 ml of 36% concentrated hydrochloric acid and 7.5 ml of isopropyl alcohol was added dropwise, and the pH was adjusted to 2.5, crystallization, crystalline 45min filtration, and then purified with 30 ml of purification water After drying temperature 55 ° C, dried under -0.090 MPa, 5 to 10 hours, to moisture less than 2.0%, resulting in pale yellow powd...

Embodiment 2

[0030] Example 2: In a 500 ml of four-mouth flasks, 20 g of cefradoxamic acid and 200 ml of purified water were added, and the temperature of 25 ° C to 30 ° C was added, and the mixture was mixed well, and the aqueous solution of 3 mol / L ammonia was added to 7.0 to 7.5, stirred for 5 min. After 6 g of ceftriaciacin C to acerase, the pH was continued with 3 mol / L ammonia solution to maintain at 7.0 to 7.5, and the reaction was completed when the pH was maintained for 5 minutes, then filtered, filtered, filtered to the cefosporin C to acerase , Collect filtrate;

[0031]When the above filtrate temperature was 10 to 15 ° C, a mixed solution of 6 ml of 36% concentrated hydrochloric acid and 6 ml of ethanol was added dropwise, and the pH was adjusted to crystalline, crystalline 45min was filtered, and then purified with 20 ml of purification, after washing, The drying temperature was 50 ° C, and the vacuum dried under -0.095 MPa was dried for 5 to 10 hours, and the water was less t...

Embodiment 3

[0032] Example 3: In a 500 ml of four-mouth flasks, 20 g of cefide sodium cefotaxime sodium celaroxime sodium and 240 ml of purified water were added, and the temperature of 25 ° C ~ 30 ° C was controlled, and the mixture was mixed well, and the aqueous solution of 3 mol / L ammonia was added to 7.0 to 7.5, stirred for 5 min. After the addition of 8 g of ceftriaridin C-deacetylase, the pH was continued with 3 mol / L ammonia solution, and the reaction was maintained at 7.0 to 7.5, and the reaction was completed when the pH was maintained for 5 minutes, then filtered, filtered, and filtered to the cefosporin C to aceralase. , Collect filtrate;

[0033] When the above filtrate temperature was 10 to 15 ° C, 4 ml of 85% phosphoric acid and a mixed solution composition of 8 ml of methanol were added dropwise, and the pH was adjusted to crystalline, crystalline 45min, filtered, then purified with 25 ml, after drying The temperature was 60 ° C, and the vacuum dried under -0.085MPa was dr...

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Abstract

The invention discloses a preparation method of 3-hydroxymethyl cefotaxime. The preparation method is characterized by comprising the following steps: adding cefotaxime into purified water at normal temperature, adjusting the pH value, then adding cephalosporin C deacetylase, filtering out the cephalosporin C deacetylase when the pH value is kept unchanged, collecting filtrate, dropwise adding a mixed solution of inorganic acid and an organic solvent, adjusting the pH value for crystallization, and performing filtering and drying after crystal growing to obtain the 3-hydroxymethyl cefotaxime.According to the preparation method, the cefotaxime is used as a raw material, a biological enzyme method is adopted, a chemical synthesis mode is avoided, the types of solvents are few, the method islow in toxicity and environmentally friendly, the reaction conditions are mild, the steps are simple, the product conversion rate is high, and the operation is simple and easy to control. The yield of a target product can reach 74%, and the purity can reach 97.6% at most. The blank of preparing the impurities by a biological enzyme method synthesis means is filled, subsequent structural analysisand pharmacological research are facilitated, and the method has important theoretical significance and practical application value for improving the quality of cefotaxime sodium, reducing the risk ofclinical medication and the like.

Description

Technical field [0001] The present invention relates to biological and pharmaceutical raw materials and intermediates, and more particularly to synthesis preparation methods of impurity 3-hydroxymethyl cefitimes in cefosporoxime sodium quality studies. Background technique [0002] Cefotaxime sodium is a third generation of hemocystin, its chemical name is (6R, 7R-3 - [(acetyloxy) methyl] -7 - [(2-amino-4-thiazole) Base) - (methoxy) ethimine group] -8-oxo-5-thio-1-nitrozible bicyclic ring [4.2.0] -2-ethyl-2-formate salt, this medicine was made of Germany Hoechst and French Roussel jointly developed successfully in 1977, in 1980, the product of the powder needles is Claforan, with a small spectrum, high efficiency, soreness, and poisonous side effects. Clinical application in various sensitive bacteria Infection treatment. [0003] In the synthetic route of the cefosporothoxime sodium domestic and foreign, most of the 7-ACA is initiated as the starting material, and the AE active ...

Claims

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Application Information

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IPC IPC(8): C12P35/02C07D501/34C07D501/12
CPCC12P35/02C07D501/34C07D501/12Y02A50/30
Inventor 雷影孙收杰陈芳芳赵威朱敬华
Owner 河北合佳创新医药科技有限公司
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