摘要
以2,4-戊二酮和三溴吡啶盐为原料合成了3-溴-2,4-戊二酮。探讨了合成过程中原料摩尔比、反应介质、反应温度、反应时间等因素对产物收率的影响,获得较佳合成条件:n(2,4-戊二酮)∶n(三溴吡啶盐)=1.2∶1,反应介质为二氯甲烷,反应温度45℃,反应时间1.5h,产品收率达92.5%。目标产物结构经红外光谱(FT-IR)、元素分析、核磁共振氢谱(~1H NMR)和核磁共振碳谱(^(13)C NMR)测定和结构表征。此方法具有操作简单、环境友好、产率高的特点。
3-Bromo-2,4-pentanedione was synthesized from 2,4-pentandione and pyridinium bromide perbromide salt. The effects of the reaction material ratio, medium, temperature and time on the yield of the product were investigated. The optimum reaction condi-tions were obtained ：ratio of 2,4-pentanedione to pyridinium bromide perbromide1. 2 ： 1 ,the dichloromethane as solvent, 1. 5 h of reaction time under the reaction temperature 45^. The yield under this optimum reaction conditions was up to 92. 5%. The struc-ture of the target product was confirmed by elementary analysis,FT-IR,1H NMR and 13C NMR spectroscopy. This method had ad-vantages of simple work-up procedure,eco-friendly and high yield.
出处
《化学研究与应用》
CSCD
北大核心
2017年第12期1868-1871,共4页
Chemical Research and Application
基金
青海大学2016年专业核心课程建设项目(2016ZYHXKC09)资助
