3, 3′-O xybis (d im ethoxyt rityl chloride)(O-DMTCl) was synthesized as a novel, acid-labile bifunctional protecting reagent. The reactions of O-DMTCl with base-protected ribonucleosides afforded unexpectedly 2′, 5′-cyclic protected ribonucleosides in addition to the expected 3′, 5′-cyclic protected ribonucleosides in good yields.