Jump to main content
Jump to site search

Issue 3, 2017
Previous Article Next Article

Continuous-flow synthesis of fluorine-containing fine chemicals with integrated benchtop NMR analysis

Author affiliations

Abstract

A compact lab plant was designed for the continuous-flow synthesis of fluorine-containing compounds and was combined with an NMR analysis platform based on a benchtop NMR spectrometer. The approach of a unified synthesis and analysis strategy for fine chemicals was applied to three different reactions, all employing fluorine as a chemical probe for online-19F NMR analysis. A high temperature synthesis for the deprotection of a CF2H group was done as well as Ruppert–Prakash reactions for the perfluoroalkylation of benzaldehyde as a model substrate. The C–H arylation of furan with a trifluoromethylated aryldiazonium salt was performed as an example of a photochemically catalyzed reaction. All three reaction classes challenge the synthesis and analysis setup differently according to sample preparation (premagnetization of bubble-free sample) and spectrometer sensitivity (signal to noise ratio, spectral resolution, scan number, substrate concentration and flow rate), but nonetheless prove the successful application of the continuous-flow synthesis of fluorinated fine chemicals with integrated online NMR analysis.

Graphical abstract: Continuous-flow synthesis of fluorine-containing fine chemicals with integrated benchtop NMR analysis

Back to tab navigation

Supplementary files

Article information


Submitted
20 Feb 2017
Accepted
14 Mar 2017
First published
24 Mar 2017

React. Chem. Eng., 2017,2, 315-323
Article type
Paper

Continuous-flow synthesis of fluorine-containing fine chemicals with integrated benchtop NMR analysis

T. H. Rehm, C. Hofmann, D. Reinhard, H. Kost, P. Löb, M. Besold, K. Welzel, J. Barten, A. Didenko, D. V. Sevenard, B. Lix, A. R. Hillson and S. D. Riegel, React. Chem. Eng., 2017, 2, 315
DOI: 10.1039/C7RE00023E

Social activity

Search articles by author

Spotlight

Advertisements