摘要
目的合成一种新的水溶性水合鸢尾异黄酮磺化衍生物[K(H2O)](C17H13O6SO3),并确定其分子结构。方法在60℃条件下用浓H2SO4磺化30 min,得到尼泊尔鸢尾异黄酮磺化物,并用体积比为1/1的乙醇-水溶液培养单晶,采用X-射线四圆衍射、IR和元素分析等方法表征其结构。结果和结论将尼泊尔鸢尾异黄酮在60℃用浓硫酸磺化,高选择性地在底物B环的3′位引入一个磺酸基,合成了水溶性尼泊尔鸢尾异黄酮衍生物,产率为82%。该合成方法简单,反应条件温和,选择性高,产物容易分离,且产率较高,是合成标题化合物一种理想的方法。X-射线晶体结构表明该化合物属于单斜晶系,空间群P2m1,晶胞参数a=0.835(4)nm,b=0.728(3)nm,c=3.000(14)nm,β=96.09(7)°,V=1.814(15)nm3,Dc=1.650 g.cm-3,Z=4。在化合物的晶体结构中,相邻的钾离子之间被O6,O7和O8桥链形成聚八面钾离子链。此外,化合物中还存在多个氢键,这使化合物自组装成一个三维网格结构的超分子。
Aim To synthesize a new hydrate potassium 5-（5, 7-dihydroxy-6-methoxy-4-oxo-4H- chromen-3-yl）-2-methoxybenzenesulfonate （[K （ H2O） ] （C17H13O6SO3 ） ） and determine its structure. Methods The new water-soluble irisolidone sulfonated derivative was synthesized by sulfonation with concentrated sulfuric acid at 60 ℃ for half an hour and the single-crystals were obtained in ethanol-water（ V/W =1/1）. The structure of the product was identified by four-circle x-ray diffractometer, IR and elemental analysis. Results and Conclusion After highly selective introduced a -SO3^- group at C3＇ on B ring of the substrate, the new water-soluble irisolidone sulfonated derivative, hydrate potassium 5-（5, 7-dihydroxy-6-methoxy-4-oxo-4H-chromen-3-yl）-2-methoxy- benzene-sulfonate, was obtained in good yield（82%） at moderate conditions. This method is an ideal synthesis way because of its simple operation, mild reaction conditions, high selectivity, easy separation of product and higher yield. The X-ray crystallography shows that the compound crystallizes in monoclinic crystal system, the space group of it is P 21/m with α= 0.835（4） nm, b=0. 728（3） nm, c=3. 000（14） nm, β= 96.09（7）°, V =1. 814（15） nm^3, Dc =1. 650 g · cm^-3 and Z =4. In the structure of the title compound, two adjacent potassium cation are bridged by O（6）, O（7） and O（8） to form a polyoctahedra potassium chain. Meanwhile, the hydrogen bonds exist in the compound, which link it to assemble a three-dimensional network structure.
出处
《宝鸡文理学院学报（自然科学版）》
CAS
2009年第3期34-39,共6页
Journal of Baoji University of Arts and Sciences(Natural Science Edition)
基金
Supported by the Natural Science Foundation of the Education Depart ment of Shaanxi Province(No.05JK136)
