13183-79-4Relevant articles and documents
Preparative Synthesis of 1,3-Dialkyltetrazolium-5-thiolates from 1-Alkyltetrazole-5-thiols
Araki, Shuki,Hirashita, Tsunehisa,Kurabayashi, Hideaki,Murakami, Suguru,Shoji, Takuo
, p. 2956 - 2961 (2022/02/07)
Mesoionic 1,3-dialkyltetrazolium-5-thiolates can be prepared in good yields by alkylation of 1-alkyltetrazole-5-thiols with secondary alcohols in concentrated sulfuric acid. The thiolates are transformed into the corresponding olates through S-alkylation followed by hydrolysis. The olates were found to be liquid at room temperature and to work effectively as polar solvents. The use of a smaller amount of sulfuric acid led to drastically different products; S-bridged dimers linked by 1,2-dimethylethylene were formed as the major products.
Antibiotic-improved cefmenoxime hydrochloride synthesis process
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Paragraph 0039-0041, (2021/02/06)
The invention discloses an antibiotic-improved cefmenoxime hydrochloride synthesis process, which comprises the following steps: step 1, preparation of 1-methyl-5-sulfydryl-1H-tetrazole, step 2, preparation of 2-(2-amino-4-azolyl)-2(Z)-methoxyimino ethyl acetate; step 3, preparation of 2-(2-amino-4-thiazolyl)-2-(Z)-methoxyimino acetic acid; step 4, preparation of 2-(2-amino-4-thiazolyl)-2-(Z)-methoxyimino acetic acid-2-benzothiazole thioester; step 5, preparation of 7-amino-3-(1-methyl-1H-tetrazole-5-thiomethyl)cephalosporanic acid hydrochloride (7-ACA-MMT. HC1); and step 6, preparation of cefmenoxime hydrochloride; domestic raw materials are adopted, the raw materials are cheap and easy to obtain in the synthesis route, the synthesis cost is reduced, and synthesis is improved; the improved process has the advantages of low raw material cost, simplicity in operation and suitability for industrial production.
Synthesis method of 1-methyl-5-mercaptotetrazole
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Paragraph 0018; 0020-0029, (2020/12/30)
The invention relates to a synthesis method of 1-methyl-5-mercaptotetrazole. The method comprises the following steps: (1) carrying out reflux reaction by using sodium methylamino dithiocarboxylate and sodium azide as reaction raw materials, water as a reaction solvent and an alkaline solution as a catalyst, neutralizing the reaction solution with a protonic acid after the reaction until the pH value is 6-7, and filtering to obtain a 1-methyl-5-mercaptotetrazole crude product; and (2) recrystallizing the 1-methyl-5-mercaptotetrazole crude product obtained in step (1) by using a recrystallization solution to obtain the 1-methyl-5-mercaptotetrazole finished product, wherein the recrystallization solution is a mixed solution of toluene and water. The synthesis method disclosed by the invention is high in yield, and the prepared 1-methyl-5-mercaptotetrazole is high in purity.