A practical, efficient and general method was developed for the deprotection of acetals/ketals to their corresponding diols R1CH(OH)CH(OH)R2 [R1 = H, CH2OH, CO2Me, CH2C(O)OMe; R2 = H, CH2OH, CO2Me, CH2OTBDPS] and catechols I [R3 = H, CO2Me; R4 = H, F, NHCbz, etc.; R5 = H, 3-NCC6H4C(O)NH, 2-Br-5-MeOC6H3C(O)NH, pyridine-3-carbonylamino, quinoline-3-carbonylamino, 1,3-benzodioxole-5-carbonylamino; R4R5 = (CH)4] using thiol immobilized on silica gel. This was an application for the well-known com. solid-supported thiol (SiliaMetS Thiol). The procedure was mild and amenable to scale-up. It does not require inert atm. and clean conversions were observed This method was applicable to substituted 1,3-benzodioxole and aliphatic acetals with different functionalities. It offered the advantage of general, green route with high yield, which could be undertaken at ambient temperature