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1-环丙基-6,7-二氟-1,4-二氢-8-甲氧基-4-氧代-3-喹啉硼二乙酯的合成研究
引用本文:周勇,郝二军.1-环丙基-6,7-二氟-1,4-二氢-8-甲氧基-4-氧代-3-喹啉硼二乙酯的合成研究[J].化学世界,2008,49(9).
作者姓名:周勇  郝二军
作者单位:1. 新乡学院化学与化工学院,河南,新乡,453003
2. 河南师范大学化学与环境科学学院,河南,新乡,453002
摘    要:用螯合法把化合物1-环丙基-6,7-二氟-1,4-二氢-8-甲氧基-4-氧代-3-喹啉羧酸乙酯(DFQ-Et)螯合制得硼螯合物(1-环丙基-6,7-二氟-1,4-二氢-8-甲氧基-4-氧代-3-喹啉羧硼二乙酯)DFQ-B(OAc)2],并考察了此步反应在DMF、DMSO等不同溶媒以及不同温度和不同时间时的反应情况。筛选结果显示,此步缩合反应的溶媒采用DMSO,所得产物(粗品)的纯度可达到大于90.0%(HPLC归一法)。总收率92.4%。该工艺反应条件温和,原料易得,操作简便,产率高,成本较低,适合工业化生产。

关 键 词:1-环丙基-6  7-二氟-1  4-二氢-8-甲氧基-4-氧代-3-喹啉硼二乙酯  硼螯合物  合成

Study on Synthesis of 1-Cyclopropyl-6,7-difluoro-8-methyl 1,4-dihydro-4-oxoquinoline Boron Diethyl Carboxylate
ZHOU Yong,HAO Er-jun.Study on Synthesis of 1-Cyclopropyl-6,7-difluoro-8-methyl 1,4-dihydro-4-oxoquinoline Boron Diethyl Carboxylate[J].Chemical World,2008,49(9).
Authors:ZHOU Yong  HAO Er-jun
Abstract:A novel synthetic route of 1-cyclopropyl-6,7-difluoro-8-methyl-1,4-dihydro-4-oxoquinoline boron diethyl carboxylate(DFQ-B(OAc)_2) was developed.The synthesis of DFQ-B(OAc)_2) from 1-cyclopropyl-6,7-difluoro-8-methyl-1,4-dihydro-4-oxoquinoline-3-diethyl carboxylate(DFQ-Et) was successful by using the boric coordination complex.The target compound was obtained by chelation method.The reaction in different solvents,under different temperature or at different time was also discussed.The results showed that DMSO was the best solvent.The purity reached was above 90.0% and the total yield rate was 92.4%.The method has the advantages of mild condition,simple operation,easy isolation,high yield rate,secure,convenient and environmental benignity.It is suitable for industrialization.
Keywords:1-cyclopropyl-6  7-difluoro-8-methyl-1  4-dihydro-4-oxoquinoline boron diethyl carboxylate  boric coordination complex  synthesis
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