2,3-二苯基-1,4,6-三氮杂二环[3.3.1]-2-壬烯单盐酸盐的合成及晶体结构

Synthesis and Crystal Structure of 2,3-Dibenzo-1,4,6-triazabicyclo[3.3.1]-2-nonenemonomuriate

在ZrOCl_2的存在下,二乙烯三氨与联苯甲酰在甲醇中回流得到2,3-二苯基-1,4,6-三氯杂二环[3.3.1]-2-壬烯单盐酸盐。对其进行了~1H NMR,IR和UV-vis谱表征及X射线单晶衍射结构分析。晶体属单斜晶系,P2_1/c空间群,晶胞参数为:a=1.69341(6)nm,b=0.77564(3)nm,c=1.21000(4)nm,β=96.1880(10)°,Z=4,D_c=1.319g·cm^(-3)。该化合物是一非平面型具有部分不饱和键的氮杂桥二环化合物,两个六元环中,与苯环连接的六元环为半椅式构型,另一六元环为椅式构型。

The azo-cycle compound, 2,3-dibenzo-1,4,6-triazabicyclo[3.3.1]-2-nonenemonomuriate, was prepared by condensation of benzil with dienthyltriamine in methanol and in the presence of ZrOCl2, and was characterized by H-1 NMR, IR and UV-vis spectra. Its crystal structure was determined by X-ray diffraction analysis. The crystal belongs to monoclinic system, space group P2(1)/c, cell parameters: a = 1.69341(6) nm, b = 0.77564(3) nm, c = 1.21000(4) nm, beta = 96.1880(10)degrees, Z = 4, D-c = 1.319 g.cm(-3). The compound is a non-planar aza-bicyclo compound with partial unsaturated bonds. The parent hexatomic ring is a chair conformation and the other six-member ring is a half-chair form.