Preparation of Grignard reagents from magnesium metal under continuous flow conditions and on-line monitoring by NMR spectroscopy

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• 作者：Michel Goldbach^a ; Ernesto Danieli^b ; Juan Perlo^c ; Bernard Kaptein^a ; Victor M. Litvinov^d ; Bernhard Blü ; mich^b ; Federico Casanova^c ; Alexander L.L. Duchateau^e ; ^{Lucien.duchateau@dsm.com" class="auth_mail" title="E-mail the corresponding author}
• 关键词：Flow NMR ; Compact NMR spectroscopy ; Grignard reaction
• 刊名：Tetrahedron Letters
• 出版年：2016
• 出版时间：6 January 2016
• 年：2016
• 卷：57
• 期：1
• 页码：122-125
• 全文大小：940 K

文摘

A convenient method for the classical preparation of Grignard reagents from aryl halides and magnesium using a fluidized bed reactor under continuous flow conditions was developed. The process was combined with quenching of the Grignard reagent by CO₂ as a model reaction performed using a second flow reactor. The formation and quenching of the reagent was monitored by on-line ¹H NMR spectroscopy. The combination of continuous flow operation for Grignard reagents with reaction monitoring by on-line NMR spectroscopy allows one to quickly optimize the working conditions.