Pentafluorophenoxyacetic acid (I) was converted to acid chloride (II) upon treatment with oxalyl chloride, and then condensed with 4'-(benzyloxycarbonyl)etoposide (III) to give diester (IV). Subsequent hydrogenolysis of the benzyloxycarbonyl protecting group of (IV) over Pd/C provided phenol (V). Finally, reaction of (V) with phosphoryl chloride, followed by aqueous work-up yielded the target phosphate.