摘要
以青霉素G钾盐与低质量分数过氧乙酸为原料氧化制备青霉素亚砜 ,其最佳工艺条件为 :n(C16 H18N2 O4 SK)∶n(CH3CO3H) =1 .0∶( 1 1～ 1 2 ) ,反应温度 0～ 5℃ ,反应时间 2 .0～ 2 5h ,w(CH3CO3H) =8 5% ,w(CH3CO2 H) =1 0 %。青霉素亚砜收率达 96 8%。同时建立了青霉素亚砜的半定量分析方法 ,以硅胶G为固定相 ,以V(CH3CO2 C4 H9 n)∶V(CH3CO2 H)∶V(NaH2 PO4 -H2 O)∶V(C4 H9OH n) =6.0∶2 .0∶1 .0∶0 5为流动相 ,用TLC法对产品进行半定量分析检测 ,并经IR、MS谱图验证了产品结构。
Penicillin G S oxide was synthesized with penicillin G and acetic hydroperoxide of low concentration.The optimal reaction conditions were as follows:mole ratio of penicillin G∶acetic hydroperoxide=1.0∶(1.1-1.2),reaction temperature 0-5 ℃,reaction time 2.0-2.5 h,concentration of acetic hydroperoxide 8 5%,concentration of acetic acid 10%.The yield of product was 96 8%.Moreover,the method of thin layer chromatography for identification of penicillin G S oxide was established with mobile phase of n butyl acetate-acetic acid-sodium dihydrogen phosphate n butanol(6.0∶2.0∶1.0∶0 5 by volume).The structure of the product was identified with IR and MS.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2000年第5期252-255,276,共5页
Fine Chemicals
基金
河北省科委资助项目! ( 972 1 3 0 52D)
关键词
青霉素
青霉素亚砜
青霉素G
抗菌素
penicillin
penicillin G S oxide
penicillin G Foundation Item:Granted by Hebei province science and technology committee(97213052D)
