摘要
以左旋磷霉素右旋苯乙胺盐为原料与氢氧化钠反应制备磷霉素钠(FS),考察了反应温度、投料时间、保温时间、氢氧化钠浓度、原料配比等因素对磷霉素钠收率的影响,并优化了磷霉素钠的析晶条件。确定适宜的合成工艺条件为:反应温度37~38℃、投料时间20min、保温时间60min、氢氧化钠浓度5mol.L-1、左磷右胺盐与氢氧化钠摩尔比1∶1.7,在此条件下,磷霉素钠的收率达85.4%。用无水乙醇在60℃、磷霉素钠投料量与乙醇用量比为1∶4(mol∶L)的条件下可析出晶型良好的磷霉素钠结晶粉末。
With phosphonomycin (R)-1-phenethylamine salt as raw material, fosfomycin sodium (FS) was prepared by reaction witl-r sodium hydroxide. The effects of various factors such as reaction temperature, feeding time,warm-keeping time, concentration of sodium hydroxide and reactant ratio on FS yield were investigated and the crystallization conditions for FS were optimized. The FS yield reached 85.4% under the optimum syn- thetic conditions as follows=the reaction temperature of 37-38℃ ,the feeding time of 20 min,the warm-keep- ing time of 60 min,the concentration of sodium hydroxide of 5 mol · L^-1 ,the molar ratio of phosphonomycin (R)-l-phenethylamine salt to sodium hydroxide was 1 : 1.7. Moreover,the FS crystal powder with good crystal type could be obtained by crystallation using anhydrous ethanol at 60 ℃ with the amount ratio of FS to ethanol of 1 : 4(mol· L).
出处
《化学与生物工程》
CAS
2013年第1期32-35,共4页
Chemistry & Bioengineering
基金
国家自然科学基金重点资助项目(20936003)
湖北省自然科学基金重点资助项目(2008CDA009)
湖北省教育厅科学技术研究项目(Q20101511)
武汉工程大学研究生创新基金项目(CX201108)
关键词
磷霉素钠
合成
工艺优化
fosfomycin sodium
synthesis
process optimization