论文部分内容阅读
经过两步反应,不经色层分离,制得了较纯净的2,9,16,23-四氨基铜酞菁和1,8,15,22-四氨基铜酞菁两种异构体.采用固相熔融催化法合成中间产物,加快反应速率;改变底物与金属盐的配比为4∶1,加适量尿素做溶剂,提高反应产率;在生成产物的还原过程中,以DMF代替水做溶剂,缩短反应时间,提高还原效率;对于产物的提纯,采取对中间产物高度提纯,通过简单的实验操作使还原充分有效,最后采取抽滤的方法,不但可以获得较纯的产物,而且简化了实验操作.对所合成的产物进行了质谱、紫外可见光谱、红外光谱表征.质谱表征的结果发现,两种异构体在其DMF溶液中都有二聚现象,而没有三聚或多聚现象,其分子上的氨基具有较强的抗氧化稳定性;紫外可见光谱表征的结果表明,前者上的氨基动力学稳定性较强,后者随着放置时间的延长,其分子上的氨基有由动力学稳定态逐渐向热力学稳定态转化的趋势,最后形成稳定的分子内氢键.
After two steps of reaction, without chromatography, the more pure 2,9,16,23-tetraaminophenanthracene and 1,8,15,22-tetraaminophenanthracene were obtained. Solid phase melting catalyst synthesis of intermediate products, to speed up the reaction rate; change the substrate and metal salt ratio of 4: 1, add appropriate amount of urea as a solvent to improve the reaction yield; In the reduction of the product, DMF instead of water As a solvent to shorten the reaction time and improve the reduction efficiency; for the purification of the product, to take a high degree of purification of intermediates, through a simple experimental operation to make full and effective reduction, and finally taken by suction filtration method, not only can be more pure product, and simplified The results of mass spectrometry showed that the two isomers were dimerized in DMF solution without trimer or poly Phenomenon, the molecular amino has strong antioxidant stability; UV-visible spectrum characterization results show that the former on the strong stability of the amino group, which with the extension of time, the molecular amino From kinetic steady state gradually to heat Steady trend of transition, the final form stable intramolecular hydrogen bonds.