3-溴-5-硝基苯基苄基醚的克级制备方法研究
Multigram scale synthesis of 3-bromo-5-nitrophenyl benzyl ether
云南民族大学学报:自然科学版,2013,22(5):327-329

杨帆 YF

摘要


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.

参考



全文: PDF      下载: 1017      浏览: 484


counter for myspace
云南民族大学学报(自然科学版) 1991—2016 Copyright
地址:云南省昆明市一二.一大街134号 邮编:650031 全国邮发代号:64-47
电话:0871-65132114 传真:0871-65137493 Email:ynmzxyxb@163.com