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Analytical Methods in Combinatorial Chemistry, Second Edition

By Bing Yan, Bin Zhang

Series Editor: Anthony W. Czarnik

CRC Press – 2011 – 238 pages

Series: Critical Reviews in Combinatorial Chemistry

Purchasing Options:

  • Add to CartHardback: $220.00
    978-0-8493-1860-3
    August 9th 2010

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.

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

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

Background

Examples

Examples: Peptide secondary structure on resin support

The monitoring of reactions on surface-functionalized polymers

Techniques

Examples

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

Author Bio

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.

Name: Analytical Methods in Combinatorial Chemistry, Second Edition (Hardback)CRC Press 
Description: By Bing Yan, Bin ZhangSeries Editor: Anthony W. Czarnik. 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...
Categories: Analytical Chemistry, Organic Chemistry, Medicinal & Pharmaceutical Chemistry