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由1,10-邻菲咯啉合成1,10-邻菲咯啉-5,6-二酮反应的副产物的形成与控制研究表明,1,10-邻菲咯啉在5,6位二酮化反应中的副反应产物及主产物分离时产生的副产物均为4,5-二氮杂芴-9-酮,二酮化反应条件(包括作为氧化剂的强混合酸H2SO4/HNO3的加入量、时间和温度)和主产物分离时体系的酸度对副产物的形成有重要影响,优化了二酮化反应条件和产物分离时的体系pH控制范围。在此优化条件下,可有效控制副产物的形成,使主产物1,10-邻菲咯啉-5,6-二酮的收率达到92%以上。
Formation and Control of By-Products of 1,10-Phenanthroline-5,6-dione Synthesized from 1,10-Phenanthroline The results showed that 1,10-phenanthroline reacted at 5,6-bis The side reaction products in the ketonization reaction and the by-products generated during the separation of the main products are 4,5-diazafluoren-9-one. The diketonation reaction conditions (including the addition of strong mixed acid H2SO4 / HNO3 as oxidant Quantity, time and temperature) and the acidity of the system when the main product is separated have an important influence on the formation of by-products, and the diketonization reaction conditions and the pH control range of the system at the time of product separation are optimized. Under the optimized conditions, the formation of by-products can be effectively controlled so that the yield of the main product 1,10-phenanthroline-5,6-dione reaches more than 92%.