摘要
本文研究了目的对合成GCLE中间体青霉素G亚砜对甲氧基苄酯的合成工艺进行改进,提高了反应收率和产物纯度。通过以青霉素G钾盐为原料,四丁基溴化铵为催化剂与对甲氧基苄基氯酯化,再与低浓度过氧乙酸氧化,采用丙酮与正己烷(体积比2:1)重结晶得到目标产物,总收率为85.5%,结果目标产物青霉素G亚砜对甲氧基苄酯通过熔点测定、1H-NMR、IR、元素分析确证其结构特征。
OBJECTIVE The synthesis process of the Intermediate of GCLE benzylpenicillin sulfoxide p-methoxybenzyl ester is improved in the article which to improve reaction yield and product purity.METHODS Benzylpenicillin potassium salt was esterified by p-methoxybenzyl chloride and catalysized by tetrabutyl ammonium bromide.then the Esterified Esters was oxidized by low concentration peracetic acid.The product was recrystallized using acetone and hexane(volume ratio of acetone to hexane was 2:1).the total yield reaches 85.5%.RESULTS The structure of benzylpenicillin sulfoxide p-methoxybenzyl ester was confirmed by melting point、1H-NMR、IR and Elemental Analysis.CONCLUSION Esterification process was added with tetrabutyl ammonium bromide of phase transfer catalyst that makes the reaction time a shorter.Using a new recrystallization sol vent makes the product a more pure.
关键词
GCLE
青霉素G亚砜对甲氧基苄酯
工艺改进
gcle
benzylpenicillin sulfoxide p-methoxybenzyl ester
process improvement