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硼氢化还原法合成二氢高红霉素硼酸酯反应条件的优化
引用本文:侯进才,刘大勇,徐启杰,时文中.硼氢化还原法合成二氢高红霉素硼酸酯反应条件的优化[J].江西师范大学学报(自然科学版),2012(1):25-28.
作者姓名:侯进才  刘大勇  徐启杰  时文中
作者单位:河南省驻马店市高级技工学校;黄淮学院化学化工系
基金项目:河南省科技发展计划重点科技攻关(092102310208)资助项目
摘    要:以红霉素亚胺醚为原料,采用硼氢化物的催化还原体系合成二氢高红霉素硼酸酯,以TLC监测反应进程,探索了反应的适宜条件,并对样品进行了表征.结果表明:以甲醇-水为反应溶剂,Pt/C(w(Pt)=1.5%)为催化剂,在红霉素亚胺醚与硼氢化钾的物质的量之比为1:7、反应温度为5℃和反应时间为6 h等条件下,二氢高红霉素硼酸酯的产率高于95%,样品符合《中国药典》和《美国药典》中二氢高红霉素硼酸酯的质量要求.

关 键 词:二氢高红霉素硼酸酯  硼氢化还原  Pt/C  催化  合成

The Optimization of Hydride Boron Reaction Conditions in Dihydro High-Erythromycin Synthesis
HOU Jin-cai,LIU Da-yong,XU Qi-jie,SHI Wen-zhong.The Optimization of Hydride Boron Reaction Conditions in Dihydro High-Erythromycin Synthesis[J].Journal of Jiangxi Normal University (Natural Sciences Edition),2012(1):25-28.
Authors:HOU Jin-cai  LIU Da-yong  XU Qi-jie  SHI Wen-zhong
Institution:1.Advanced Technical Schools,Zhumadian Henan 463000,China;2.Department of Chemistry and Chemical Engineering,Huanghuai University,Zhumadian Henan 463000,China)
Abstract:The high-dihydro erythromycin borate was synthesized from erythromycin iminoether by using cata-lytic-reduction of boron hydride,and the progress was monitoring by TCL.The reaction conditions of optimization were researched and the product was characterized.The results showed that the suitable reaction conditions were methanol-water as solvent,Pt/C(w(Pt)=1.5%) as a catalyst,molar ratio of erythromycin iminoether and potassium borohydride 1︰7,reaction temperature 5 ℃,reaction time 6 h,and the yield was above 95%.The product is ac-cording with the quality standard of Chinese Pharmacopoeia and the United States Pharmacopoeia.
Keywords:high-dihydro erythromycin borate  sodium borohydride reduction  Pt/C  catalysis  synthetic
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