喹啉杂环类中间体6-溴-4-氯-3-硝基喹啉的合成研究  

Study on the Synthesis of 6-Bromine-4-chloro-3-nitroquinoline

作　　者：李贺 祁红娇 LI He;QI Hong-jiao(Anhui Research Institute of Chemical Industry,Hefei 230041,China;Hefei IP Translation Co.Ltd.,Hefei 230071,China)

机构地区：[1]安徽省化工研究院,安徽合肥230041 [2]合肥智财专利翻译咨询有限公司,安徽合肥230071

出　　处：《安徽化工》2019年第1期79-80,84,共3页Anhui Chemical Industry

摘　　要：通过以6-溴-3-硝基-4-羟基喹啉、草酰氯为主要原料,以N,N-二甲基甲酰胺为催化剂,二氯甲烷为溶剂合成了6-溴-4-氯-3-硝基喹啉。主要考查了反应物配比、催化剂用量、反应时间和溶剂用量等因素对产物收率的影响。实验表明,优化反应条件为:n(6-溴-3-硝基-4-羟基喹啉)∶n(草酰氯)∶n(N,N-二甲基甲酰胺)=1.0∶1.5∶0.08,反应时间2 h时,收率为93.44%,质量分数达99.6%。该合成方法操作简单,环境污染少,有工业应用前景。6-Bromo-4-chloro-3-nitroquinoline was synthesized from 6-bromo-3-nitro-4-hydroxyquinoline and oxalyl chloride with the catalysis of N,N-dimethylformamide in dichloromethane.The effects of molar ratio of reactants,dosage of catalyst,reaction time and dosage of solvent on the synthesis were investigated.The optimal reaction conditions were n(oxaloyl chloride)∶n(6-bromo-3-nitro-4-hydroxyquinoline)=1.5∶1,n(N,N-dimethylformamide)∶n(6-bromo-3-nitro-4-hydroxyquinoline)=0.08∶1,and reaction time was 2 h.The yield of 6-bromo-4-chloro-3-nitroquinoline was up to 93.44%with 99.6%purity.This method is simple,safe,environmental friendly,and suitable for industrial production.

关 键 词：6-溴-3-硝基-4-羟基喹啉 草酰氯 6-溴-4-氯-3-硝基喹啉 

分 类 号：TQ251.1[化学工程—有机化工]