High resolution MAS-NMR in combinatorial chemistry

• Published in: Biotechnology and bioengineering 2000, Vol.71 (2), p.130-148
• Main Authors: Shapiro, Michael J., Gounarides, John S.
• Format: Article
• Language: English
• Subjects: 2-D NMR; combinatorial chemistry; Combinatorial Chemistry Techniques; diffusion-weighted MAS-NMR; High-resolution magic angle-spinning NMR; Magnetic Resonance Spectroscopy - methods; Molecular Conformation; on-resin reaction monitoring; Peptides - chemistry; Resins, Plant; solid-phase organic chemistry
• ISSN: 0006-3592; 1097-0290
• DOI: 10.1002/1097-0290(2000)71:2<130::AID-BIT1004>3.0.CO;2-R

High‐resolution magic angle spinning (hr‐MAS) NMR is a powerful tool for characterizing organic reactions on solid support. Because magic angle spinning reduces the line‐broadening due to dipolar coupling and variations in bulk magnetic susceptibility, line widths approaching those obtained in solution‐phase NMR can be obtained. The magic angle spinning method is amenable for use in conjunction with a variety of NMR‐pulse sequences, making it possible to perform full‐structure determinations and conformational analysis on compounds attached to a polymer support. Diffusion‐weighted MAS‐NMR methods such as SPEEDY (Spin‐Echo‐Enhanced Diffusion‐Filtered Spectroscopy) can be used to remove unwanted signals from the solvent, residual reactants, and the polymer support from the MAS‐NMR spectrum, leaving only those signals arising from the resin‐bound product. This review will present the applications of high‐resolution magic angle spinning NMR for use in combinatorial chemistry research. © 2001 John Wiley & Sons, Inc. Biotechnol Bioeng (Comb Chem) 71:130–148, 2000/2001.