知识与财富的链接
报道了3-溴-5-硝基苯基苄基醚的制备方法 .苄醇对3,5-二硝基溴苯的芳香亲核取代反应极易受后续副反应的影响,对反应中碱、溶剂、浓度、温度、反应时间和投料量等因素进行了系统的研究,发现在DMF中50℃下与苄醇和叔丁醇钾反应10 min可以高产率得到克级目标产物.反应体系的颜色变化可作为判断反应终点的指标.
A practical multi-gram scale synthesis of 3-bromo-5-nitrophenyl benzyl ether was developed.The aromatic nucleophilic substitution of benzyl alcohol to 1-bromo-3,5-dinitrobenzene was found highly sensitive to the following side reactions.After a detailed evaluation of the reaction parameters,including the base,solvent,concentration,temperature,time,and reaction scale,the research found the target product could be obtained reliably at the multi-gram scale by stirring it with benzyl alcohol and potassium tert-butoxide in DMF at 50℃ for several minutes.The color change of the reaction system was found an accurate indicator of the end of this reaction.