以苄氯和诺氟沙星为原料,无水碳酸钾和碘化钾为催化剂,采用微波辐射技术合成了诺氟沙星衍生物,产品结构经IR和1HNMR分析证明与预期结构相符;同时运用正交试验对影响收率的因素进行考察,确定了最佳反应条件:微波辐射功率700W,辐射时间15 ...以苄氯和诺氟沙星为原料,无水碳酸钾和碘化钾为催化剂,采用微波辐射技术合成了诺氟沙星衍生物,产品结构经IR和1HNMR分析证明与预期结构相符;同时运用正交试验对影响收率的因素进行考察,确定了最佳反应条件:微波辐射功率700W,辐射时间15 m in,反应温度80℃,苄氯、诺氟沙星和碳酸钾的物质的量比为1.3∶1∶1,碘化钾用量0.3 g;反应收率也从常规加热法的29.3%提高到90.2%.与常规加热法对比,微波法缩短了反应时间,提高了反应收率.展开更多
The properties of norfloxacin(NFX)and its 4?-N-acetyl derivative(ANFX)are investigated in different pH aqueous solutions and H2O-CH3CN mixed solutions,to determine the effects of pH and polarity on their ground and ex...The properties of norfloxacin(NFX)and its 4?-N-acetyl derivative(ANFX)are investigated in different pH aqueous solutions and H2O-CH3CN mixed solutions,to determine the effects of pH and polarity on their ground and excited states.The triplet states of NFX and ANFX are affected more by pH than by polarity.The pH dependence of the NFX and ANFX triplet states is likely due to the different quantum yields of different protonated forms.Steady-state fluorescence,time-resolved fluorescence,and laser flash photolysis experiments at different pH values provide clear evidence of the involvement of different intramolecular charge-transfer pathways in the singlet states of NFX and ANFX.The different electron-donating capacities of 1-N,1?-N,and 4?-N under different conditions determine the major pathway.展开更多
文摘以苄氯和诺氟沙星为原料,无水碳酸钾和碘化钾为催化剂,采用微波辐射技术合成了诺氟沙星衍生物,产品结构经IR和1HNMR分析证明与预期结构相符;同时运用正交试验对影响收率的因素进行考察,确定了最佳反应条件:微波辐射功率700W,辐射时间15 m in,反应温度80℃,苄氯、诺氟沙星和碳酸钾的物质的量比为1.3∶1∶1,碘化钾用量0.3 g;反应收率也从常规加热法的29.3%提高到90.2%.与常规加热法对比,微波法缩短了反应时间,提高了反应收率.
基金supported by the National Natural Science Foundation of China(10675158)
文摘The properties of norfloxacin(NFX)and its 4?-N-acetyl derivative(ANFX)are investigated in different pH aqueous solutions and H2O-CH3CN mixed solutions,to determine the effects of pH and polarity on their ground and excited states.The triplet states of NFX and ANFX are affected more by pH than by polarity.The pH dependence of the NFX and ANFX triplet states is likely due to the different quantum yields of different protonated forms.Steady-state fluorescence,time-resolved fluorescence,and laser flash photolysis experiments at different pH values provide clear evidence of the involvement of different intramolecular charge-transfer pathways in the singlet states of NFX and ANFX.The different electron-donating capacities of 1-N,1?-N,and 4?-N under different conditions determine the major pathway.
