Guo Ya-ning
2009
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Journal
Journal of Baoji University of Arts and Sciences
Abstract
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.