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Impurity Detection in Solid-Phase Organic Chemistry: Scope and Limits of HR MAS NMR

✍ Scribed by Pierre Rousselot-Pailley; Delphine Maux; Jean-Michel Wieruszeski; Jean-Louis Aubagnac; Jean Martinez; G Lippens

Book ID
104202790
Publisher
Elsevier Science
Year
2000
Tongue
French
Weight
99 KB
Volume
56
Category
Article
ISSN
0040-4020

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✦ Synopsis

AbstractÐWe evaluate the possibilities and limits of HR MAS NMR to detect and quantify side products during solid-phase synthesis, using a model system where pyroglutamate and glutamate are coupled in a well de®ned ratio. Resins swollen in deuterated and protonated solvent are studied. Use of the LED sequence eliminates the peaks due to the use of protonated solvents, but sensitivity is decreased, and differential losses of magnetization might lead to a biased population estimation. However, as all sample workup steps are eliminated, this technique will be helpful in detecting minority species in solid-phase combinatorial chemistry, and its application at the different steps of the reaction might lead to the early detection of otherwise unidenti®able active components.

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