- New adaptation diseases of cefoperazone medicinal preparation for treating endometritis and other gynecological genital tract infections
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The invention discloses new adaptation diseases of cefoperazone medicinal preparation for treating gynecological genital tract infections of gynecology department. The cefoperazone sodium provided bya specific raw material production process is extremely low in impurity content and remarkable in medicine effect, so that the quality of a preparation product is improved, the safety and effectiveness of the preparation product are guaranteed, and the invention provides the application of preparing the medicine for treating endometritis and other gynecological genital tract infections.
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Paragraph 0108; 0110-0111
(2020/08/22)
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- Preparation method of cefoperazone acid
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The invention relates to a preparation method of cefoperazone acid. The preparation method comprises the following steps: (1) in a dichloromethane system, allowing 7-TMCA to react with a silanizationreagent at 20-70 DEG C, and carrying out silanization protection on the amino group and the carboxyl group; (2) in a dichloromethane body and a DMA system, allowing HO-EPCP salt to react with ethyl chloroformate at the reaction temperature of 20-70 DEG C under the action of a catalyst to prepare mixed anhydride; (3) adding the 7-TMCA after silanization protection into the mixed anhydride, reactingat 20-70 DEG C to obtain a reaction solution; (4) hydrolyzing the reaction solution, adding alkali to adjust the pH to be 5.5-7.5, layering, adding solvent into the water phase, adding acid to adjustthe pH to be 1.5-2.5, crystalizing and filtering to obtain cefoperazone acid. The method disclosed by the invention has the advantages that the product yield can be improved, S-isomer can be reduced,the residual solvent is reduced, the solvent is easy to recycle, the wastewater does not contain phosphorus and is easy to process.
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Paragraph 0024; 0025; 0026; 0027; 0028
(2019/01/06)
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- Process for the preparation of keto acid [...]
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The invention belongs to the field of medicine, and particularly relates to a preparation method of cefoperazone acid. The method comprises the following steps: with 7-ACA (amin-oeephalosporanic acid) and 1-methyl-5-tetrazole-thione as raw materials under catalysis of boron trifluoride acetonitrile, reacting to prepare 7-TMCA (7-Amino-3-[[(1-methyl-1H-tetrazol-5-yl)thio]methyl]-3-cephem-4-carboxylicacid)hydrochloride; carrying out carboxyl and amino group protection on the 7-TMCA hydrochloride by using trimethylchlorosilane; and with the group-protected 7-TMCA hydrochloride prepared in the step (1), HO-EPCP ((2R)-2-[(4-Ethyl-2,3-dioxopiperazinyl)carbonyllamino]-2-(4-hydroxyphenyl)acetic acid) and benzotriazole diethyl phosphonate as raw materials, carrying out N-acylation reaction in a DMF (Dimethyl Formamide) solution under catalysis of triethylamine, so as to obtain the cefoperazone acid, wherein acyl chloride is prepared by reaction in absence of the HO-EPCP, the benzotriazole diethyl phosphonate is directly added to directly carry out acylation reaction on the HO-EPCP and the group-protected 7-TMCA hydrochloride. Thus, the preparation method is simple in reaction step, low in cost and high in purity.
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Paragraph 0026; 0028
(2017/03/14)
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- Synthetic method of cefoperazone acid
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The invention discloses a synthetic method of cefoperazone acid. The method comprises the steps of: reacting raw materials of 7-ACA and 1-methyl-5-mercapto tetrazole under the catalysis of boron trifluoride acetonitrile to obtain 7-ACT; dissolving the 7-ACT in a mixed solution of acetonitrile and N,O-(bis) trimethylsilyl acetamide to obtain a 7-ACT amino alkylate solution; mixing HO-EPCP, an organic solvent and a catalyst, adding phosphorus oxychloride for reaction at the temperature of -25 to -20 DEG C, wherein when the residue amount of HO-EPCP in the reaction solution is no more than 0.5%, the reaction is complete, so as to prepare a HO-EPCP acyl chloride solution; mixing and reacting 7-ACT amino alkylate solution with HO-EPCP acyl chloride solution, adding an aqueous solution of sodium bicarbonate after the reaction, standing foe stratification, filtering a lower layer material, adding water, crystallizing, filtering, washing and drying to obtain the cefoperazone acid. The method has the advantages of simpleness, high yield and stable intermediate.
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- NOVEL CRYSTALLINE CEFOPERAZONE INTERMEDIATE
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The present invention relates to a crystalline form of an intermediate for cefoperazone of formula (1) and to a process for the preparation thereof by enzymatic condensation of a 3′-thiosubstituted β-lactam nucleus with a phenylglycine derivative.
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Paragraph 0063
(2015/04/28)
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- Dioxo piperazine compounds
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Certain cephalosporins having a heterocyclicthiomethyl group at the 3-position such as cefoperazone are prepared by reacting a solution of a 7-acylamidocephalosporanic acid having a free amino group as part of said acyl substituent with about an equi-molar amount of the thiolester STR1 wherein --S-Het is the desired conventional heterocyclicthio group which displaces the 3-acetoxy group of the starting acid and STR2 is the conventional acyl group which displaces a hydrogen on the free amino group which is part of the acyl substituent of the starting 7-acylamidocephalosporanic acid.
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