响应面法优化Beckmann重排反应制备苯甲酰苯胺

Optimization of Beckmann Rearrangement by Response Surface Method to Prepare Benzoylaniline

为研究不同催化剂对Beckmann重排反应性能的影响,以二苯甲酮为原料制备二苯甲酮肟,利用Beckmann重排制得苯甲酰苯胺.用单因素和响应面法对影响重排反应的因素如催化剂种类、催化剂用量、催化剂比例、反应温度及反应时间进行优化.结果表明:催化剂为磷酸∶乙酸酐=2∶3,催化剂用量4mL,反应时间30min,反应温度120℃时,催化效果最好.对制得的苯甲酰苯胺进行红外光谱、核磁共振分析和表征,结果表明该法具有操作简便、产率高等优点.

To study the effect of different catalysts on the Beckmann rearrangement reaction,the Benzophenone was used as the starting material to synthesize the target compound Benzanilide by Beckmann rearrangement reactions.Parameters that influence the Beckmann rearrangement such as the types of catalyst,catalyst dosage,catalyst ratio,reaction temperature and reaction time were investigated by single-factor experiment or response surface methodology.The optimized synthetic conditions were:phosphoric acid-acetic anhydride(2/3,v/v)as catalyst,4 mL as the catalyst dosage,120℃as the reaction temperature and 30 min as the reaction time.In addition,the reaction product of Benzanilide was confirmed by means of infrared spectroscopy and nuclear magnetic resonance.The results indicate that this method has the advantages of simpler operation and higher yield.