Development of a Process for the Preparation of Chloromethyl Chlorosulfate

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• 作者：Bin Zheng ; Masano Sugiyama ; Martin D. Eastgate ; Alan Fritz ; Saravanababu Murugesan ; David A. Conlon
• 刊名：Organic Process Research & Development
• 出版年：2012
• 出版时间：November 16, 2012
• 年：2012
• 卷：16
• 期：11
• 页码：1827-1831
• 全文大小：204K
• 年卷期：v.16,no.11(November 16, 2012)
• ISSN：1520-586X

文摘

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 provides an efficient and scalable protocol for the preparation of CMCS in 92% solution yield and high purity (>99 GC area %).