A novel solid-phase phosphoramidite based oligodeoxynucleotide two-step synthesis methodhas been developed. Keys to this method are replacement of the 5'-dimethoxytrityl blocking group with anaryloxycarbonyl and the use of N-dimethoxytrityl protection for the exocyclic amines of adenine and cytosine.With these modifications, coupling of each 2'-deoxynucleoside 3'-phosphoramidite to the growingoligodeoxynucleotide on the solid support can be followed by treatment with an aqueous mixture of peroxyanions buffered at pH 9.6. This reagent effectively removes the carbonate protecting group andsimultaneously oxidizes the phosphite internucleotide linkage. As a consequence a new two-step synthesiscycle is possible. Oligodeoxynucleotides synthesized using this approach are identical to authentic sampleswhen tested by a variety of analytical techniques.