We report on our findings concerning the microwave-assisted silica gel removal of Boc and t-Bu groups protecting ?-NH₂ and COOH groups in amino acids and peptides, and also on selectivity of this deprotection to OH-protecting t-Bu groups. To obtain high conversions in deprotection, increased microwave doses and prolongation of the reaction time are required. As a consequence, relatively large amounts of side products were detected. The microwave radiation could possibly be utilized in deprotection of peptides when the trifluoroacetic acid cleavage and subsequent neutralization of the acid with a tertiary base have to be avoided.