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

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.