水合鸢尾异黄酮磺化物[K（H2O）]（C17H13O6SO3）的合成及晶体结构

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P21m,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.

Synthesis and structure of hydrate potassium 5-(5,7-dihydroxy-6-methoxy-4-oxo-4H-chromen-3-yl)-2-methoxybenzenesulfonate

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/V=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 -SO- 3 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 P21m with 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 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.