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Preparation method for Cefoxintin sodium

A technology of cefoxitin sodium and cefoxitin acid, which is applied in the direction of organic chemistry, can solve the problems of low product content and high solvent residue of cefoxitin sodium, and achieve the effects of high content, good product color grade, simple and feasible method

Inactive Publication Date: 2012-04-04
苏州盛达药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The cefoxitin sodium that this method makes mainly has solvent residue high, and the defect that product content is lower

Method used

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  • Preparation method for Cefoxintin sodium
  • Preparation method for Cefoxintin sodium
  • Preparation method for Cefoxintin sodium

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preparation example Construction

[0029] See figure 1 , A method for preparing cefoxitin sodium of the present invention, the specific steps include:

[0030] (100). Preparation of acid solution: firstly mix the first solvent and the second solvent to form a mixed solution, cool to 8°C-12°C, and then add cefoxitin acid to the mixed solution to dissolve to form an acid solution. The volume ratio of the first solvent to the second solvent is 1:5-8; the first solvent is preferably methanol, and the second solvent is preferably ketone solvents such as acetone, methyl ethyl ketone, and methyl isobutyl ketone;

[0031] (200), decolorization: control the temperature T=-2~0℃, add activated carbon to the acid solution to decolorize for 25~35min to form a decolorized acid solution;

[0032] (300). Filtration and washing: pass the decolorized acid solution through a microporous filter membrane to form a filtered acid solution, pass the lye solution through the microporous filter membrane to form a filtered lye solution, and di...

Embodiment 1

[0040] (1) Add 80ml methanol and 440ml methyl ethyl ketone into a 1000ml four-neck reaction flask, cool to 10°C, add 50g cefoxitin acid, rinse the bottle wall with 200ml methyl ethyl ketone, stir to dissolve;

[0041] (2) Control the temperature T=-2-0℃, add 5g of 767 activated carbon to decolorize for 25min;

[0042] (3) Add 85ml methanol and 10ml methyl ethyl ketone into a 500ml four-necked reaction flask, add 13.5g sodium tert-butoxide at room temperature, rinse the wall of the bottle with 15ml methanol, stir to dissolve to form lye;

[0043] (4) The lye is passed through a 0.45 micron microporous membrane. This process should take about 1 min. The temperature of the filtrate is cooled to T=-2-0℃, and it is ready for use;

[0044] (5) Prepare pickling solution, mix 50ml methanol with 250ml methyl ethyl ketone, cool to T=-2-0℃, set aside;

[0045] (6) Pass the acid solution formed in step (1) through a 0.45 micron microporous membrane, and wash the carbon cake twice with the acid solu...

Embodiment 2

[0055] (1) Add 90ml methanol and 450ml acetone into a 1000ml four-necked reaction flask, cool to 10°C, add 50g cefoxitin acid, rinse the bottle wall with 210ml acetone, stir to dissolve;

[0056] (2) Control the temperature T=-2-0℃, add 5g of 767 activated carbon to decolorize for 30min;

[0057] (3) Add 75ml methanol and 10ml acetone into a 500ml four-necked reaction flask, add 11g sodium acetate at room temperature, rinse the bottle wall with 10ml methanol, and stir to dissolve;

[0058] (4) The sodium acetate solution is passed through a 0.45 micron microporous membrane. This process should take about 1 min. The temperature of the filtrate is cooled to T=-2-0°C, and it is ready for use;

[0059] (5) Prepare pickling solution, mix 40ml methanol with 250ml acetone, cool down to T=-2-0℃, set aside;

[0060] (6) Pass the acid solution formed in step (1) through a 0.45 micron microporous membrane, and wash the carbon cake twice with the acid solution formed in step (5);

[0061] (7) Combin...

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Abstract

The invention discloses a preparation method for Cefoxintin sodium. The preparation method particularly comprises the steps of preparing acidic solution, decoloring, filtering and washing, performing crystallization for the first time, cultivating a crystal, performing crystallization again, performing suction filtration and washing, and drying. The preparation method for the Cefoxintin sodium is simple and practicable. The prepared finished product has few solvent residues, high content and high color grade.

Description

Technical field [0001] The invention relates to the field of chemical pharmacy, in particular to a preparation method of cefoxitin sodium. Background technique [0002] Cefoxitin sodium, chemical name: (6R, 7S)-3-carbamoyloxymethyl-7-methoxy-8-oxo-7-[2-(2-thiazolyl) Acetamido]-5thiabicyclo[4.2.0]oct-2-ene-2-carboxylic acid sodium salt. Its chemical structure is as follows: [0003] [0004] Cefoxitin sodium is a second-generation cephalosporin antibiotic developed by Merck, USA. It has a balanced antibacterial spectrum and is stable to β-lactamase. At present, due to the increasing bacterial resistance of cephalosporins, cefoxitin, which is different from the first and third generation cephalosporins, has once again attracted people's attention. [0005] The traditional synthetic route mainly uses carboxyl protected 7-ACA as a raw material, and undergoes amino conversion, bromination, oxidization, hydrogenation reduction, and deprotection to obtain cefoxitin. The reaction route i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D501/57C07D501/04C07D501/12
Inventor 曾润保周自金王芳罗新祖
Owner 苏州盛达药业有限公司
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