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Organic synthesis on solid-phase resins requires new applications of nondes
tructive analytical tools to monitor the progress of reactions. Herein we d
escribe our novel approach to validate a five-step reaction sequence on res
in. We have developed a protocol list that allows us to follow reactions st
ep-by-step using different analytical procedures in the order of increasing
experiment time. Results from these various techniques for each reaction s
tep are contrasted and compared. The key to achieve definitive analytical d
ata for the entire reaction sequence is the combined application of more th
an one analytical technique.