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本文合成了23个2,3-二取代苯骈-1-氧-2-硫化磷-3-氮杂环已-4-酮(化合物Ⅰ)和3个2,3-二取代苯骈-1-氧-2-氧化磷-3-氮杂环已-4-硫酮(化合物Ⅱ)新的有机环磷化合物,并用红外吸收光谱、氢核磁共振谱、紫外吸收光谱、X射线衍射分析和元素分析等方法鉴定了它们的组成和结构.并研究了23个化合物Ⅰ的红外吸收光谱,发现它们在指纹区1290—1319cm~(-1)范围内均有强吸收峰.经综合分析各光谱数据和实验结果,肯定了此强峰与P=O基因吸收峰的区别,并确认为不饱和碳原子C—N键伸缩振动所造成的特征吸收。 在合成上述化合物的过程中,往往在反应溶液中得到“正常产物”Ⅰ及其同分异构体“异常产物”Ⅱ 的混合物.通过选择适宜的缩合条件,可使其中某一异构体成为主要产物,并可在合适的溶剂中经多次重结晶将它们分离.本文提供了三对此类同分异构体的融点、红外吸收光谱、紫外吸收光谱和氢核磁共振谱等方面的数据,并对各谱图作了初步解析。
In this paper, 23 2,3-disubstituted benzono-1-oxo-2-phosphosulfan-3-azacyclohexan-4-one (compound I) and 3 2,3-disubstituted benzo [ -oxo-2-phospho-3-azacyclohexan-4-thione (Compound II) was synthesized and characterized by IR, 1HNMR, UV absorption, X-ray diffraction and elemental analysis Their structures and structures were identified and analyzed by IR spectra and IR spectra of 23 compounds I were studied and found to have strong absorption peaks in the range of 1290-1319cm ~ (-1) And the experimental results, the difference between the peak of this strong peak and the P = O gene was confirmed, and the characteristic absorption caused by the stretching vibration of the C-N bond of the unsaturated carbon atom was confirmed. In the process of synthesizing the above compounds, a mixture of “normal product” I and its isomer “abnormal product” II is often obtained in the reaction solution. By selecting suitable condensation conditions, one of the isomers can be made into The major products, which can be separated by multiple recrystallizations in a suitable solvent, provide data on the melting points, infrared absorption spectra, UV-Vis spectra, and proton nuclear magnetic resonance spectra of three such isomers , And made a preliminary analysis of the various spectra.