二苯并-18-冠-6-硝化产物异构体的分离及顺式化合物的结构测定

Isomer Seperation of Dibenzo-18-Crown-6 Nitration and Structure Determination of the Cis Product

在改进的条件下,二苯并-18-冠-6硝化反应的产率达90%以上。提出一种分离二硝基二苯并-18-冠-6的顺、反异构体的方法。反应产物经元素分析和红外光谱鉴定,异角X射线衍射法测定了顺式二硝基二苯并-18-冠-6的晶体结构。晶体空间群为P21/n,α=15.95i(7)■,b=20.411(9)■,c=8.173(4)■,β=101.09(4)°,Z=4。结构用直接法解出,R=0.067。

Under the improved condition, the dibenzo-18-crown-6 can be nitrated with production rate over 90 per cent. In addition, we proposed a method by which the cis-dinitro-dibenzo-18-crown-6 can be easely separated from its trans isomer. By combining elemental analysis, infrared and X-ray diffraction results, the molecular and crystal structure of cis-dinitro-dibenzo-18-crown-6 has been determined. The crystals belong to monoclinic space group P21/n, with a= 15.985(7), 6 = 20.411(9), c = 8.173(4)■, β=101.09(4)°, Z = 4. The structure was solved by direct methods and refined to convergence with final R value of 0.067.