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(5S, 6R) cloxacillin penicilloate as well as preparation method and application thereof

A technology of cloxacillin penicillin thiazole salt and cloxacillin, which is applied in the field of drug impurity preparation, can solve problems such as unfavorable application, high impurity content in products, and great influence on finished product quality, and achieves simple and easy preparation process and high product purity. High effect with low equipment requirements

Inactive Publication Date: 2014-07-02
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the reference substance required for the detection of cloxacillin penicillin thiazole mainly refers to the preparation of penicillin thiazole or oxacillin thiazole, but the resulting product has high impurity content, which has a great impact on the quality of the finished product and is not conducive to application.

Method used

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  • (5S, 6R) cloxacillin penicilloate as well as preparation method and application thereof
  • (5S, 6R) cloxacillin penicilloate as well as preparation method and application thereof
  • (5S, 6R) cloxacillin penicilloate as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 1) Add 0.2mmol cloxacillin to a 50mL ground-mouth Erlenmeyer flask with a stopper, and then add 10mL aqueous sodium hydroxide solution with a concentration of 0.2mol / L (the amount of solute sodium hydroxide is 2mmol) to obtain colorless Clarify the transparent solution, then put the Erlenmeyer flask into a heat-collecting magnetic stirrer, stir for 60 minutes at a speed of 500 r / min in a constant temperature water bath at 25°C for alkali destruction, and obtain the cloxacillin penicillin thiazole sodium intermediate;

[0035] 2) Add hydrochloric acid with a concentration of 0.1mol / L to the obtained cloxacillin penicillin thiazole sodium intermediate until the pH value is adjusted to 8.12, seal the Erlenmeyer flask and refrigerate at 4°C for 48 hours to obtain a slightly yellowish clarification Solution; the solution is taken out and freeze-dried immediately. The specific operation of freeze-drying is to freeze in a -80°C refrigerator for 12h, then transfer to a freeze dr...

Embodiment 2

[0037] 1) Add 0.2mmol cloxacillin to a 50mL ground-necked Erlenmeyer flask with a stopper, and then add 1mL aqueous sodium carbonate solution with a concentration of 2mol / L (the amount of solute sodium hydroxide is 2mmol) to obtain a colorless, clear and transparent solution, and then put the Erlenmeyer flask into a heat-collecting magnetic stirrer, stir at a speed of 600r / min for 5min in a constant temperature water bath at 60°C for alkali destruction, and obtain the cloxacillin penicillin thiazole sodium intermediate;

[0038] 2) Add hydrochloric acid at a concentration of 1 mol / L to the obtained cloxacillin penicillin thiazole sodium intermediate until the pH value is adjusted to 6, seal the Erlenmeyer flask and place it in a water bath at 30°C for a heating reaction for 24 hours, A slightly yellow clear solution was obtained; the solution was taken out and freeze-dried immediately. The specific operation of freeze-drying was to freeze in a -70°C refrigerator for 24 hours, a...

Embodiment 3

[0040] 1) Add 0.2mmol cloxacillin to a 50mL ground-mouth conical flask with a stopper, and then add 10mL of 0.02mol / L sodium hydroxide solution in absolute ethanol (the amount of solute sodium hydroxide is 0.2mmol ), to obtain a colorless, clear and transparent solution, and then put the Erlenmeyer flask into a heat-collecting magnetic stirrer, stir at a speed of 550r / min for 30min in a constant temperature water bath at 40°C for alkali destruction, and obtain cloxacillin penicillin thiazole Sodium acid intermediate;

[0041]2) Add nitric acid with a concentration of 0.01 mol / L to the obtained cloxacillin penicillin thiazole sodium intermediate until the pH value is adjusted to 10.2, seal the Erlenmeyer flask and place it in a water bath at 40°C for heating for 56 hours , to obtain a slightly yellowish clear solution; the solution was taken out and freeze-dried immediately. The specific operation of freeze-drying was to freeze in a -75°C refrigerator for 18h, then transfer to ...

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Abstract

The invention provides a (5S, 6R) cloxacillin penicilloate as well as a preparation method and application thereof. The preparation method comprises the steps of adding an alkali solution into cloxacillin serving as a raw agent to perform alkali destroy on the cloxacillin, wherein the molar ratio of the cloxacillin to the solute in the alkali solution is 1: (1-10); adding an acid solution to adjust the pH value of the solution to be 6-10.2, then reacting, and freeze-drying the solution obtained by the reaction to obtain the (5S, 6R) cloxacillin penicilloate. The preparation method is simple, convenient, feasible, simple in operation, mild in reaction conditions, low in equipment requirement, cheap and readily available in raw materials, low in cost, high in yield and high in product purity and is an economic and efficient method for preparing the (5S, 6R) cloxacillin penicilloate, and the prepared (5S, 6R) cloxacillin penicilloate can be applied to the detection of cloxacillin antibiotics.

Description

technical field [0001] The invention belongs to the field of pharmaceutical impurity preparation, and specifically relates to (5S, 6R) cloxacillin penicillin thiazole salt and a preparation method and application thereof. Background technique [0002] Cloxacillin (also known as cloxacillin, cloxacillin) is an acid-resistant and enzyme-resistant isoxazole semi-synthetic penicillin antibiotic. It is a derivative of 6-aminopenicillanic acid (6-APA). Acid resistance to penicillinase is significantly better than other antibiotics, and will not be destroyed by penicillinase in vivo. Cloxacillin sodium plays an important role in those patients who are refractory to penicillin G therapy. Its bactericidal activity is strong, and its mechanism of action is mainly to achieve curative effect by inhibiting the replication and synthesis of cell wall. Cloxacillin is widely used in the treatment of cow mastitis and other diseases because of its low price, convenient use and obvious antiba...

Claims

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Application Information

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IPC IPC(8): C07D417/12G01N30/02G01N30/90G01N21/3563
CPCC07D417/12G01N21/3563G01N30/90G01N2030/025G01N2500/20
Inventor 傅强孙敏杜康丽杜玮蔡刚常春
Owner XI AN JIAOTONG UNIV
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