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Process for preparing instantly-dissolving cefmenoxime hydrochloride

A technology of cefmenoxime hydrochloride and a preparation process, which is applied in the field of preparation of instant cefmenoxime hydrochloride, can solve the problems of increased workload of hospital nurses, increased difficulty of sub-packaging work, increased production workers, etc., and shortens the dissolution time and facilitates the The effect of sub-packaging and reducing labor intensity

Active Publication Date: 2010-06-16
桂林澳林制药有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the first method has brought unnecessary troubles to the hospital and increased the workload of the nurses in the hospital; the second method has added a work procedure to the production workers, and increased the difficulty of the packaging work, and in this Significantly increased chance of visible foreign matter in the process

Method used

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  • Process for preparing instantly-dissolving cefmenoxime hydrochloride

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preparation example Construction

[0018] The preparation technology of instant type cefmenoxime hydrochloride of the present invention comprises the following steps:

[0019] 1) Take the crude product of cefmenoxime hydrochloride and add water to prepare a suspension, add sodium carbonate to dissolve it, and obtain a clarified liquid;

[0020] 2) Decolorize the clarified liquid with activated carbon, wash with water, and combine the washing liquids to obtain solution A;

[0021] 3) Adjust the pH value of solution A to 0.8-1.2 with hydrochloric acid, filter, collect the filtrate, and obtain solution B;

[0022] 4) Adjust the pH of solution B to 1.3-1.75 with a weak alkaline solution, stir for crystallization, filter after complete crystallization, wash with water, and dry in vacuum to obtain the product.

[0023] In order to improve the yield of the product, the residue filtered in step 3) can also be washed with hydrochloric acid with a pH value of 0.8 to 1.2, the acid washing solution is collected, and the c...

Embodiment 1

[0032] 1, the preparation of cefmenoxime hydrochloride of the present invention:

[0033] 1) 10Kg of cefmenoxime hydrochloride crude product was dissolved in 200L of water to prepare a suspension, and 1.8Kg of sodium carbonate was added under stirring to dissolve it to obtain a clear solution;

[0034] 2) Decolorize the clarified liquid with activated carbon, filter, wash the carbon layer with water, and combine the washing liquids to obtain solution A;

[0035] 3) Adjust the pH value of solution A to 1.0 with 2mol / L hydrochloric acid, filter, collect the filtrate, and obtain solution B;

[0036] 4) adjust the pH value of solution B to 1.3 with an aqueous solution of sodium carbonate with a mass concentration of 10%, stir and crystallize at room temperature, after most of the crystals are separated out, then maintain this temperature and stir and crystallize for 2 hours, filter, and wash the crystals with water first, then Wash with 95% (v / v) ethanol and dry in vacuum to obta...

Embodiment 2

[0054] 1, the preparation of cefmenoxime hydrochloride of the present invention:

[0055]1) 10Kg of cefmenoxime hydrochloride crude product was dissolved in 200L of water to prepare a suspension, and 1.8Kg of sodium carbonate was added under stirring to dissolve it to obtain a clear solution;

[0056] 2) Decolorize the clarified liquid with activated carbon, filter, wash the carbon layer with water, and combine the washing liquids to obtain solution A;

[0057] 3) Use 2mol / L hydrochloric acid to adjust the pH value of solution A to 1.0, filter, collect the filtrate, wash the residue with an aqueous hydrochloric acid solution with a pH value of 1.0, collect the aqueous hydrochloric acid washing solution, combine the filtrate and the acid washing solution, and obtain solution B;

[0058] 4) adjust the pH value of solution B to 1.4 with an aqueous solution of sodium carbonate with a mass concentration of 20%, stir and crystallize at room temperature, after most of the crystals ar...

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Abstract

The invention discloses a process for preparing instantly-dissolving cefmenoxime hydrochloride, which comprises the following steps: 1) adding water into a coarse product of cefmenoxime hydrochloride to prepare a suspension, adding sodium carbonate into the suspension to dissolve the cefmenoxime hydrochloride, and thus obtaining clear liquor; 2), decolorizing the clear liquor by using active carbon, washing the clear liquor and mixing the washing liquor to obtain solution A; 3) adjusting the pH value of the solution A to 0.8 to 1.2 by using hydrochloric acid, filtering the solution A and collecting the filtrate to obtain solution B; and 4), adjusting the pH value of the solution B to 1.3 to 1.75 by using an alkalescent solution, stirring the solution B for crystallization, filtering the solution after the crystallization is finished, washing crystals and drying the crystals under vacuum to obtain the instantly-dissolving cefmenoxime hydrochloride. Compared with the prior art, the method has the advantages that: the pH value is adjusted at two stages and the crystallization is performed under a condition of a pH value of 1.3 to 1.75, so the precipitated crystals have a proper particle size and good dispersibility, can be charged conveniently and separately and can dissolve in a short time; the operation process is simplified; the risks of producing visible foreign matters are reduced greatly; the production efficiency is improved; the cost is reduced; and the clinic use and operation are convenient.

Description

technical field [0001] The invention relates to a preparation process of instant cefmenoxime hydrochloride, which belongs to the technical field of chemical pharmacy. Background technique [0002] Cefmenoxime is the third-generation cephalosporin for injection developed by Japan's Takeda Pharmaceutical Co., Ltd. It was first launched in Japan in 1983 and entered the latest editions of European and American pharmacopoeias. Currently used mainly is its hydrochloride form, i.e. cefmenoxime hydrochloride, its chemical name is [6R-[6α, 7β(Z)]]-7-[[(2-amino-4-thiazolyl)( Methoxyimino)acetyl]amino-3-[[(1-methyl-1H-tetrazol-5-yl)thio]methyl]-8-oxo-5-thia-1-azadi Cyclo[4,2,0]oct-2-ene-2-carboxylate hydrochloride, the molecular formula is C16H17N9O5S3 1 / 2HCl, the molecular weight is 529.79, and its chemical structure is as follows: [0003] [0004] Cefmenoxime hydrochloride is mainly used for the treatment of various inflammations caused by bacterial infections. Its antibacteria...

Claims

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Application Information

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IPC IPC(8): C07D501/36C07D501/12
Inventor 黄文豪崔志宏周艺海
Owner 桂林澳林制药有限责任公司
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