摘要
以六甲基二硅烷、7-氨基头孢烷酸(7-ACA)、2,3-环戊烯并吡啶及苯并噻唑活性酯(AEME)为主要原料合成了头孢匹罗硫酸盐。首先六甲基二硅烷与碘在氮气保护下合成了三甲基碘硅烷(TMeSiI),不需分离,TMeSiI直接与7-ACA和2,3-环戊烯并吡啶反应得到了头孢匹罗主重要中间体(7-ACP),其次,7-ACP与AEME在三乙胺存在下合成了头孢匹罗,最后以乙醇作结晶溶剂用20%的硫酸酸化得到头孢匹罗硫酸盐。实验中,考查了影响反应的主要因素,确定了反应的最优条件,并通过元素分析、1HNMR对中间体7-ACP和头孢匹罗硫酸盐进行了表征。
Cefpirome sulfate was synthesized by using hexamethyldisiliane, 7-aminocephalosporanic acid (7-ACA), 2,3-cyclopenteno pyridine and AEME as main raw material. Firstly, trimethyliodosiliane (TMeSiI) was obtained by reacting hexamethyldisiliane with iodine under nitrogen protection, and TMeSiI was treated with 2,3-cyclopenteno pyridine and 7-ACA to give a significant intermediate product (7-ACP) of cefpirome. Secondly, cefpirome was synthesized from 7-ACP and AEME under triethylamine. Finally, using ethanol as crystal solvent, cefpirome sulfate was obtained by acidifying cefpirome with 20% sulfuric acid. In the experiment, the primary factors affecting on the reaction were studied. The optimum conditions were determined. The structure of 7-ACP and cefpirome sulfate was characterized by the element analysis and 1 HNMR.
出处
《石油化工高等学校学报》
CAS
2003年第3期29-33,共5页
Journal of Petrochemical Universities
