摘要
以青霉素G钾为原料,与对硝基氯苄在DMF中酯化制得青霉素G对硝基苄酯,再用过氧化氢-乙酐氧化,制得头孢菌素类新型母核原料GCLE(7-苯乙酰胺基-3-氯甲基头孢烯酰酯)的中间体青霉素G亚砜对硝基苄酯。确定了最佳酯化反应条件:反应温度50-50℃,反应时间3 h。确定了最佳氧化反应条件:青霉素G钾/过氧化氢摩尔比为1:3,反应温度0℃,反应体系pH值为4-5,反应时间3 h。实验结果表明,该法反应条件易于控制,反应收率达82.4％。
A phenethylpenicillin sulfoxide 4 - nitrobenzyl ester,intermediate for new material GCLE (7 - phenylac-etamido - 3 - chloromethyl cephalosorinate) of cephalosporin antibiotics, was synthesized by the esterification of phenethylpenicillin G potassium with 4 - nitrobenzyl chloride in DMF and the oxidation of phenethylpenicillin 4 -nitrobezyl ester with peroxide of hydrogen in acetic anhydride. The optimum conditions of esterification were determined as follows: reaction temperature 50-55℃, and reaction time 3 h. The optimum conditions of oxidation were determined as follows: reaction temperature 0℃, pH value of reaction system 4-5 , and reaction time 3 h. The result showed that the reaction conditions were easy to be controlled and overall yield was up to 82.4% .
出处
《精细石油化工进展》
CAS
2004年第2期53-55,共3页
Advances in Fine Petrochemicals
