Efficient Transposition of the Sandmeyer Reaction from Batch to Continuous Process

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• 作者：Joseph D’Attoma ; Titi Camara ; Pierre Louis Brun ; Yves Robin ; Stéphane Bostyn ; Frédéric BuronSylvain Routier
• 刊名：Organic Process Research & Development
• 出版年：2017
• 出版时间：January 20, 2017
• 年：2017
• 卷：21
• 期：1
• 页码：44-51
• 全文大小：453K
• ISSN：1520-586X

文摘

The transposition of Sandmeyer chlorination from a batch to a safe continuous-flow process was investigated. Our initial approach was to develop a cascade method using flow chemistry which involved the generation of a diazonium salt and its quenching with copper chloride. To achieve this safe continuous process diazotation, a chemometric approach (Simplex method) was used and extrapolated to establish a fully continuous-flow method. The reaction scope was also examined via the synthesis of several (het)aryl chlorides. Validation and scale-up of the process were also performed. A higher productivity was obtained with increased safety.