Analytical Methods in Combinatorial Chemistry  book cover
2nd Edition

Analytical Methods in Combinatorial Chemistry

ISBN 9781138116689
Published June 14, 2017 by CRC Press
238 Pages 70 B/W Illustrations

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Book Description

Since the publication of the benchmark first edition of this book, chemical library and combinatorial chemistry methods have developed into mature technologies. There have also been significant shifts in emphasis in combinatorial synthesis. Reflecting the growth in the field and the heightened focus on select areas, Analytical Methods in Combinatorial Chemistry, Second Edition updates a classic text and captures the current state of these technologies.

Written by leaders in the field, this second edition includes several enhancements. A chapter on high-throughput analytical methods and informatics reflects the demand for quality control of library members. A new chapter focuses on high-throughput purification methods. All chapters have been updated with new data.

Topics discussed in this second edition include:

  • Properties of solid-phase samples, analytical studies targeted to understand these properties, and resin swelling
  • Fourier Transform Infrared techniques
  • On-support mass spectrometry and nuclear magnetic resonance methods used in the reaction optimization stage
  • Combinatorial library analysis using spectrophotometric, fluorometric, and other methods
  • Quality control of combinatorial libraries
  • High-throughput purification methods
  • Future directions and analytical challenges

The coming decade is sure to usher in a new wave of progress in this critical field. This volume provides not only an analysis of the recent developments in analytical methods, technologies and applications; it also provides a window on future possibilities.

Table of Contents

Analytical issues in combinatorial chemistry
Combinatorial chemistry
Synthesis methods
Analytical challenges
Properties of solid supports
Reaction Optimization Stage
Library synthesis stage
Lead selection and optimization stage

An examination of the analytical sample: resin support
Physical properties of resins
Resin type
Resin bead size distribution
Loading and the intraresin site distribution
Thermal stability
Chemical stability
Resin swelling and solvation
Effects of swelling on resin
Effects of swelling on reagent and solvent molecules
Swelling ability of solvents
Dynamic resin solvation
Effects of the solvated resin on solid-phase reactions
The effects of support solvation on SPPS
Resin support as another "solvent phase"
Support effects on SPOS reaction kinetics
Site separation and site interaction
Solid support effects on product purity

Solid-phase reaction optimization using FTIR
Comparison of FTIR and Raman techniques
Analysis of resin-bound compounds
Comparison of techniques
Monitoring of polymer-supported organic reactions
The monitoring of reactions on polystyrene-based resin
Yes-and-no information
Reaction kinetics on resin support
Quantitative estimation of chemical conversions (%) on resin
The selection of optimal reaction conditions using single-bead IR
The monitoring of reactions on PS-PEG resins: comparing the reaction rate on PS and PS-PEG resins
Examples: Peptide secondary structure on resin support
The monitoring of reactions on surface-functionalized polymers
Parallel reaction monitoring

Reaction optimization using MS and NMR methods
MS methods
NMR methods
Gel-phase NMR
Magic angle spinning (MAS) NMR
Other NMR methods

Reaction optimization using spectrophotometric and other methods
Qualitative analysis of amines
Quantitative analysis of amines
Quantitative spectroscopic methods for organic functional groups
Quantitation of aldehyde/ketone groups
Quantitation of hydroxyl groups on resin
Quantitation of carboxyl groups on resin
Quantitation of polymer-supported sulfhydryl groups
Combustion elemental analysis methods
Analysis of resin-bound organic compounds
Quantitatively monitoring SPOS reactions
Electrochemical methods
On-resin X-ray, EPR, SERS, and fluorescence methods

Quality control of combinatorial libraries
Analysis of discrete compound libraries
MS analysis
MS-guided purification
High-throughput NMR
Analysis of pooled libraries
Theoretical calculation of mass distribution
MS analysis
High-resolution MS
Tandem MS
Liquid chromatography (LC)/MS and capillary electrophoresis (CE)/MS
NMR methods for mixture analysis
HPLC for analyzing compounds from discrete and mixture libraries
HPLC with a chemiluminescence nitrogen detector (CLND)
Evaporative light scattering detector (ELSD)

High-throughput purification
Nonchromatographic high-throughput purification methods
Chromatographic high-throughput purification methods
Supercritical fluid chromatographic purification methods
Purification methods based on fluorous chemistry separation technique
Fluorous liquid–liquid extraction (F-LLE)
Fluorous solid-phase extraction (F-SPE)
Fluorous HPLC (F-HPLC)
Fluorous-flash chromatography (F-FC)

Final Thoughts and Future Perspectives
Stability of compound collections
Nano-combinatorial library and associated analytical issues
Green process and technologies

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Bing Yan received his Ph.D. from Columbia University with Koji Nakanishi in 1990. He is a faculty member at the Department of Chemical Biology and Therapeutics at St. Jude Children’s Research Hospital in Memphis, Tennessee, and an adjunct professor at Shandong University.

Bin Zhang received his Ph.D. from the Institute of Inorganic and Analytical Chemistry and Radiochemistry at Saarland University (Germany) with Professor Doctor Horst P. Beck in 2003. He is an associate professor of analytical chemistry in the School of Chemistry and Chemical Engineering at Shandong University, China.