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机构地区:[1]山西阳煤丰喜肥业(集团)有限责任公司,山西运城044100
出 处:《化工中间体》2013年第9期54-56,共3页
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
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