KR960034206A - Method for preparing cephalosporin intermediate - Google Patents

Method for preparing cephalosporin intermediate Download PDF

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Publication number
KR960034206A
KR960034206A KR1019950007076A KR19950007076A KR960034206A KR 960034206 A KR960034206 A KR 960034206A KR 1019950007076 A KR1019950007076 A KR 1019950007076A KR 19950007076 A KR19950007076 A KR 19950007076A KR 960034206 A KR960034206 A KR 960034206A
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KR
South Korea
Prior art keywords
dimethylaminoethyl
tetrazol
amino
carboxylic acid
preparing
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Application number
KR1019950007076A
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Korean (ko)
Inventor
신준섭
라영준
강복구
Original Assignee
김종인
영진약품공업 주식회사
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Application filed by 김종인, 영진약품공업 주식회사 filed Critical 김종인
Priority to KR1019950007076A priority Critical patent/KR960034206A/en
Publication of KR960034206A publication Critical patent/KR960034206A/en

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Abstract

본 발명은 세포티암 및 그 에스테르의 함성에 유용한 중간체인 7β-아미노-3-Ⅱ1-(2-디메틸아미노에틸)-1Ⅱ-테트라졸-5-일[티오메닐]-세프-3-엠-4-카르복실산 1/2황산염의 제조방법을 제공하며, 이방법은 7β-어미노세팔로스포린산과 5-머르캅토-1-(2-N,N-디메틸아미노에틸)-1Ⅱ-테트라졸을 황산 존재하 유기용매와 산무수물 존재하에 반응시키고, 이어 반응 혼합물을 알콜류로 희석하여 염기로 pⅡ를 조정하여 결정로 얻는것을 특징으로 한다.The present invention relates to 7β-amino-3-II1- (2-dimethylaminoethyl) -1II-tetrazol-5-yl [thiomenyl] -sef-3-m-, which is an intermediate useful for the containment of cytothioma and its esters. Provided is a method for preparing 4-carboxylic acid 1/2 sulfate, which comprises 7β-aminocephalosporinic acid and 5-mercapto-1- (2-N, N-dimethylaminoethyl) -1II-tetrazole. The reaction mixture is reacted in the presence of sulfuric acid in the presence of an organic solvent and an acid anhydride, and then the reaction mixture is diluted with alcohols to adjust pII with a base to obtain crystals.

Description

세팔로스포린 중간체의 제조방법Method for preparing cephalosporin intermediate

본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음Since this is an open matter, no full text was included.

Claims (5)

다음 구조식(Ⅳ)의 7β-아미노세팔로스포린산과 구조식(Ⅴ)의 5-머르캅토-1-(2-N,N-디메틸아미노에틸)-1Ⅱ-테트라졸을 유기용매와 황산중에서 20~50도로 반응시켜서 직접 구조식(Ⅱ)의 7β-아미노-3-Ⅱ1-(2-디메틸아미노에틸)-1Ⅱ-테트라졸-5-일[티오메닐]-세프-3-엠-4-카르복실산 1/2 황산염을 제조하는 방법.7β-aminocephalosporinic acid of formula (IV) and 5-mercapto-1- (2-N, N-dimethylaminoethyl) -1II-tetrazole of formula (V) in 20-50 Reaction of the reaction mixture to directly 7β-amino-3-II1- (2-dimethylaminoethyl) -1II-tetrazol-5-yl [thiomenyl] -cep-3-m-4-carboxylic acid of structural formula (II) Method for preparing 1/2 sulphate. 제1항에 있어서, 초산 무수물을 첨가하여 사용하므로서 무수조건을 강화시키는 구조식(Ⅱ)이 7β-아미노-3-Ⅱ1-(2-디메틸아미노에틸)-1Ⅱ-테트라졸-5-일[티오메닐]-세프-3-엠-4-카르복실산 1/2황산염의 제조방법.The structural formula (II) according to claim 1, wherein the anhydrous condition is enhanced by adding acetic anhydride is 7β-amino-3-II1- (2-dimethylaminoethyl) -1II-tetrazol-5-yl [thiomethol]. Nil] -sef-3-em-4-carboxylic acid 1/2 sulfate. 제1항에 있어서, 반응용매로 니트릴류, 니트로알칸류, 유기산류, 케톤류, 에테르류와 설폴린등을 사용하는 구조식(Ⅱ)의 7β-아미노-3-Ⅱ1-(2-디메틸아미노에틸)-1Ⅱ-테트라졸-5-일[티오메닐]-세프-3-엠-4-카르복실산 1/2황산염의 제조방법.The 7β-amino-3-II1- (2-dimethylaminoethyl) of formula (II) according to claim 1, wherein nitriles, nitroalkanes, organic acids, ketones, ethers and sulfolines are used as reaction solvents. A process for preparing -1II-tetrazol-5-yl [thiomenyl] -sef-3-m-4-carboxylic acid 1/2 sulfate. 제1항에 있어서, 침전용매로 메탄올, 에탄올, 이소프로판올등의 알콜류를 사용하는 구조식(Ⅱ)의 7β-아미노-3-Ⅱ1-(2-디메틸아미노에틸)-1Ⅱ-테트라졸-5-일[티오메닐]-세프-3-엠-4-카르복실산 1/2황산염의 제조방법.The 7β-amino-3-II1- (2-dimethylaminoethyl) -1II-tetrazol-5-yl of Structural Formula (II) using alcohols such as methanol, ethanol and isopropanol as precipitation solvents. Method for preparing thiomenyl] -sef-3-m-4-carboxylic acid 1/2 sulfate. 제1항에 있어서, 반응후 침전시 트리에틸아민, 디메틸아민등의 유기염기나 무기염기를 이용하여 중화하므로서 결정성 구조식(Ⅱ)의 7β-아미노-3-Ⅱ1-(2-디메틸아미노에틸)-1Ⅱ-테트라졸-5-일[티오메닐]-세프-3-엠-4-카르복실산 1/2황산염의 제조방법.2. The 7β-amino-3-II1- (2-dimethylaminoethyl) of the crystalline structure (II) according to claim 1, wherein the precipitate is neutralized using an organic base or an inorganic base such as triethylamine, dimethylamine, or the like after precipitation. A process for preparing -1II-tetrazol-5-yl [thiomenyl] -sef-3-m-4-carboxylic acid 1/2 sulfate. ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.※ Note: The disclosure is based on the initial application.
KR1019950007076A 1995-03-30 1995-03-30 Method for preparing cephalosporin intermediate KR960034206A (en)

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KR1019950007076A KR960034206A (en) 1995-03-30 1995-03-30 Method for preparing cephalosporin intermediate

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KR1019950007076A KR960034206A (en) 1995-03-30 1995-03-30 Method for preparing cephalosporin intermediate

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100432425B1 (en) * 2000-11-16 2004-05-22 씨제이 주식회사 Novel method for preparation of cephem derivatives or salts thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100432425B1 (en) * 2000-11-16 2004-05-22 씨제이 주식회사 Novel method for preparation of cephem derivatives or salts thereof

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