74769-12-3Relevant academic research and scientific papers
Synthetic method of cefoperazone acid
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Paragraph 0013; 0014; 0015; 0016; 0017, (2016/11/17)
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.
A convenient synthesis of crystalline 4-ethyl-2,3-dioxopiperazine-1- carboxamido-p-hydroxyphenylacetyl chloride using triphosgene
Wei, Wen-Long,Li, Jun-Bo,Xin, Yang,Chang, Hong-Hong,Li, Yan-Wei
experimental part, p. 328 - 329 (2009/06/25)
The crystalline 4-ethyl-2,3-dioxopiperazine-1-carboxamido-p- hydroxyphenylacetyl chloride was prepared in 97.6% yield when triphosgene was reacted with D(-)-2-[(4-ethyl-23-dioxo-1-piperazineyl)-carbonylamino]-2-(4- hydroxyphenyl)acetic acid (HO-EPCP) in methylene dichloride at 0～5°C in the presence of triethylamine (TEA). This new method without using chlorinating agent such as phosgene, diphosgene, phosphorus oxychloride or oxalyl chloride enjoys a number of advantages in that the reaction is carried out under mild conditions and is clean.
