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 relia- bly at the multi - gram scale by stirring it with benzyl alcohol and potassium tert - butoxide in DMF at 50℃ for sev- eral minutes. The color change of the reaction system was found an accurate indicator of the end of this reaction.
出处
《云南民族大学学报(自然科学版)》
CAS
2013年第5期327-329,共3页
Journal of Yunnan Minzu University:Natural Sciences Edition
基金
国家自然科学基金(81173029)
云南省自然科学基金(2010ZC016)
关键词
3-溴-5-硝基苯基苄基醚
芳香亲核取代
克级制备
3 -Bromo-5 -nitrophenyl benzyl ether
aromatic nucleophilic substitution
multi -gram scale synthesis