一水合羟苯磺酸钙的制备及结构分析

Synthesis and structural analysis of calcium dobesilate monohydrate

目的 制备一水合羟苯磺酸钙并进行结构鉴定。方法 在不加溶剂的情况下,直接用浓硫酸磺化对苯二酚再与CaCO3成盐,在一定条件下脱水制得了产物一水合羟苯磺酸钙,产物结构经IR, 1H -NMR, 13C NMR,MS,TGA,DSC及粉末X 衍射确证。结果 精制品在1. 33kPa, 80℃下干燥4h,得本品一水合物。TGA,DSC及粉末X 射线衍射表明,本品一水合物与二水合物谱图完全不同。结论 简化了反应操作,提高了反应收率,减少了环境污染。

OBJECTIVE To synthesize calcium dobesila te monohydrate and to confirm its chemical structure.METHOD Calcium dobesilate was synthesized by sulfonation of hyd roquinone with H 2SO 4 without using any solvent. Calium dobesilate monohydrat e was obtained under given conditions and its chemical structure was identified by IR,、 1H-NMR, 13CNMR, MS,TGA,DSC and powder X-ray diffraction etc.RESULTS The purified product was dried under 1.33kPa and 80℃ t o give its monohydrate. TGA showed loss of weight at 100～180℃ is 4.19%, DSC sh owed dehydrate starting at 134℃ and ending at 180℃ and 2 nd endothermal p rocess occurring at 212℃ with no mass variation. Powder X-ray diffraction anal ysis indicated the monohydrate is different from the dihydrate.CONCLUSION The synthetic route was simplized and the overall yi eld was raised, pollution of the environment was reduced.