Process understanding and optimization either with DoE or kinetic modeling, kinetic repeatability studies, QbD assessments of API reaction conditions, etc. are all critical procedures. However, have users thought about utilizing NMR for these protocols? NMR solves problems more quickly and with higher confidence because of its quantitative nature and ability to provide unprecedented structural information.
Bruker offers InsightXpress, the latest stopped-flow solution dedicated for monitoring reactions by NMR. It can be used for screening many different reaction conditions rapidly, which significantly increases productivity. Even time consuming and labor-intensive kinetic studies that were previously performed by standard NMR tube procedure are now rapidly screened.
When it comes to understanding fast reactions, Bruker’s InsightXpress again provides the ideal solution. It integrates rapid sample/reaction delivery with the NMR’s analytical power. A better understanding about the kinetics and mechanism of rapid chemical reactions, which are yet to be understood, is now at the users’ fingertips.
- Direct quantitative and comprehensive structural data from only a single analytical method
- Reaction understanding – unique insights into the mechanisms of chemical reactions
- Quick screening of reaction conditions
- Unparalleled speed to monitoring the rapid depletion of reagents with half-life of less than 1 second
- Automatic experiment set-up is possible even in fully protonated solvents
- Fast and easy set-up
- Used when required, seats on SampleXpress base (compatible with open access system)
- Unlimited shots
- Low volumes of sample (600 μL/shot)
- Accurate temperature control (enables complete kinetics studies)
- Variable ratios of reagents to investigate different reaction conditions
- Accurate timing using a trigger pulse
- Pre-magnetization volume for three different reagents (accurate quantitative information)
- Dead-time less than 150 ms, allowing the monitoring of rapid reactions
- Reproducible with stable quantified volume
- In-situ cleaning through dedicated solvent flush line
- Fast flow-rate injection (0.2 – 2 ml/second)
- Easy automatic optimization of NMR parameter
- Compatible with all Bruker 5 mm probes
- Intuitive software for data acquisition and analysis
As a stopped–flow solution, the InsightXpress features a temperature controlled transfer line, a pumping unit, and a flow tube and software. The system can be easily set-up in Bruker’s high-resolution NMR spectrometers with protected magnets (300-700 MHz). The InsighMRTM software from Bruker makes data acquisition and analysis simple and easy and is equipped with a novel functionality that allows for the monitoring of extremely fast reactions.
Optimization of Suzuki-Miyaura Coupling
In organic chemistry, especially in the pharmaceutical industry, Suzuki-Miyaura couplings are among the most utilized reactions but the reaction and side reactions are yet to be fully understood. Bruker’s InsightXpress enabled Professor Lloyd-Jones and colleagues to gain a better understanding of the reaction mechanism of extremely fast protodeboronation, i.e., Suzuki-Miyaura side reaction.(1,2) The InsightXpress helped them to track the decay of a reagent with half-life time of approximately one second. They observed the reaction at various conditions of pH, concentration and temperature (0-70 °C).
- Cox PA, Reid M, Leach AG, Campbell AD, King EJ, Lloyd-Jones GC, J Am ChemSoc, in Press, DOI: 10.1021/jacs.7b07444
- Cox PA, Reid M, Leach AG, Campbell AD, Lloyd-Jones GC, J Am ChemSoc, 138, 9145-57 (2016)
About Bruker BioSpin - NMR, EPR and Imaging
Bruker BioSpin offers the world's most comprehensive range of NMR and EPR spectroscopy and preclinical MRI research tools. The Bruker BioSpin Group of companies develop, manufacture and supply technology to research establishments, commercial enterprises and multi-national corporations across countless industries and fields of expertise.
Bruker microCT formerly known as SkyScan develops and produces wide range of high-end microtomography instruments for life science, material research and in-vivo preclinical studies.
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