作者:Bin Zheng、Masano Sugiyama、Martin D. Eastgate、Alan Fritz、Saravanababu Murugesan、David A. Conlon
DOI:10.1021/op300246d
日期:2012.11.16
A new and efficient synthesis of chloromethyl chlorosulfate (CMCS) from chloroiodomethane and chlorosulfonic acid is described. This process leverages a chlorosulfonic acid-mediated iodide oxidation to drive the equilibrating displacement process to full conversion. The resulting iodine byproduct is further oxidized and removed as iodate, to prevent iodide-induced decomposition of CMCS. This new process
描述了一种由氯碘甲烷和氯磺酸新型高效合成氯甲基氯硫酸盐(CMCS)的方法。该方法利用氯磺酸介导的碘化物氧化来驱动平衡置换过程至完全转化。将所得的碘副产物进一步氧化并以碘酸盐形式除去,以防止碘化物诱导的CMCS分解。这一新工艺以92%的溶液收率和高纯度(> 99 GC面积%)为制备CMCS提供了有效且可扩展的方案。