An efficient synthetic method of nucleoside-5′-(1-hydroxymethylene-1, 1-bisphosphonates) is reported here. The procedure was optimized with 3′-protected thymidine and then applied to synthesis of new AZT analogues. We thank Pr. J. Liquier from the Laboratoire de Chimie Structurale Biomoléculaire (UMR 7033-CNRS, Bobigny, France) for IR spectra, the Laboratoire de Biochimie des Protéines et Protéomique (UPRES EA 3408, Bobigny, ...