Radiation-induced reactions in chemically amplified resists based on deprotection of t-butoxycarbonyl groups have been investigated by both time-resolved (the pulse radiolysis methods) and steady-state optical absorption spectroscopy. Upon exposure of a partially tBOC-protected novolak by electron and synchrotron radiation beams, the yields of the intermediates contributing to the acid generation (phenoxyl radical and proton adducts of base resin) decreased with increasing the protection ratio of hydroxyl groups. Therefore, the efficiency of the acid generation is closely related with the protection ratio. The relation of the acid generation mechanism with the protection ratio was discussed.