MAS NMR technique with standard equipment was used to characterize the intermediate products in a three step reaction scheme leading to disubstituted olefins on solid support. The step-by-step analysis of the reaction presented here demonstrates that the goal of reaction characterization and optimization in situ can be obtained in an entirely satisfying manner using conventional MAS NMR. Some of the experimental parameters that should be taken into consideration to obtain workable spectra are examined. Copyright (C) 1996 Elsevier Science Ltd