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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。
OBJECTIVE To synthesize a new water-soluble hydrated iris sulfonated derivative [K (H2O)] (C17H13O6SO3) and determine its molecular structure. Methods Sulfonated with concentrated H2SO4 at 60 ℃ for 30 min, the isoflavone sulfonates of Nepalsia japonica were obtained. The single crystals were cultured in ethanol - water solution of 1/1 volume ratio and characterized by X - ray diffraction, IR and elemental analysis Method to characterize its structure. Results and Conclusion The Nepalsii iris isoflavones were sulfonated with concentrated sulfuric acid at 60 ° C and a sulfonic acid group was introduced at the 3 ’position of the B ring of the substrate selectively to synthesize a water-soluble Nephelium isoflavone derivative in a yield of 82%. The synthesis method is simple, the reaction conditions are mild, the selectivity is high, the product is easily separated, and the yield is high, which is an ideal method for synthesizing the title compound. The X-ray crystal structure indicates that the compound belongs to the monoclinic system with space group P2m1. The unit cell parameters a = 0.835 (4) nm, b = 0.728 (3) nm, c = 3.000 ) °, V = 1.814 (15) nm3, Dc = 1.650 g.cm-3, Z = 4. In the crystal structure of the compound, adjacent potassium ions are formed into polybasic potassium ion chains by O6, O7 and O8 bridge chains. In addition, there are multiple hydrogen bonds in the compound, which make the compound self-assemble into a three-dimensional lattice structure of supramolecules.