甲磺司特的合成

Synthesis of suplatast tosilate

目的优化甲磺司特合成路线及工艺条件,使其适合工业生产。方法以环氧氯丙烷为起始原料经过醚化和环合"一锅法"、再醚化、催化氢化、酰化、成盐5步反应合成了甲磺司特。结果合成得到目标产物,纯度大于99%,总收率37.2%,产物经MS1、H-NMR、IR、元素分析等方法确证了结构。结论与文献报道的路线相比,本研究较详细考察了合成工艺,摸索出了最佳的投料方式,优化了原料配比,缩短了反应时间,简化了合成工艺。

Objective To optimize the synthetic route of suplatast tosilate to make it suitable for industrial production. Methods Epichlorohydrin was used as starting material and adopted hydrocarbylation and cyclization by one-pot method, followed with re-hydrocarbylation, catalytic hydrogenation, acylation, and salt formation to afford suplatast tosilate. Results The target compound was synthesized, with its purity more than 99 % and the total yield of 37.2 %. The structure of the product was elucidated by MS, 1^H-NMR, IR and elemental analysis. Conclusion Compared with the synthesis route that had been reported in the literature, the synthesis route in this study was optimized by exploration of optimization of the Molar ratio of raw materials, shortening of the reaction time, and simplification of synthesis route.