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目的合成比卡鲁胺有关物质B并测定其理化性质。方法以1,2-环氧-2-甲基-N-[4-氰基-3-(三氟甲基)苯基]丙酰胺为起始原料,经缩合、氧化两步反应制得N-[4-氰基-3-(三氟甲基)苯基]-3-(3-氟苯硫酰基)-2-甲基-2-羟基丙酰胺(比卡鲁胺有关物质B),用IR、1H-NMR、13C-NMR、质谱、元素分析及差热分析对其结构进行表征,使用UV和DSC对其在不同溶剂中的溶解度和熔点进行分析。结果合成总收率达到74.6%,纯度为99.58%。通过溶解度的测定说明其在醇酮等有机溶剂中有一定的溶解度,但在不同pH值的水介质中几乎不溶。结论本合成方法操作简单、反应条件温和,能容易地制备比卡鲁胺有关物质B,在此基础上测定的物化数据可为相关研究提供有益参考。
Objective To synthesize bicalutamide-related substance B and determine its physico-chemical properties. Methods Starting from 1,2-epoxy-2-methyl-N- [4-cyano-3- (trifluoromethyl) phenyl] propionamide by condensation and oxidation, - [4-Cyano-3- (trifluoromethyl) phenyl] -3- (3- fluorophenylthio) -2-methyl-2- hydroxypropanamide (Bicalutamide Related Substance B) Its structure was characterized by IR, 1H-NMR, 13C-NMR, MS, elemental analysis and differential thermal analysis, and its solubility and melting point in different solvents were analyzed by UV and DSC. Results The total yield of synthesis reached 74.6% with a purity of 99.58%. The determination of solubility shows that it has some solubility in organic solvents such as alcohol ketones, but it is almost insoluble in aqueous media with different pH values. Conclusion The method is simple and can be used to prepare bicalutamide related substance B easily. The physicochemical data determined on the basis of this method can provide useful reference for the related research.