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Solid-phase synthesis using pent-4-enoyl nucleoside (PNT) phosphonamidites allow for the facile preparation of oligonucleoside methylphosphonates, methylphosphonothioates and their chimeric analogs. WithPNT phosphonamidites, nucleobase and phosphate deprotection, as well as, cleavage from the support can all be accomplished by treatment of the support-bound oligonucleotide with NH 4 OH (28%, rt, 1 h).