Chemical synthesis of 2'-O-[13C]methyl-rCGCGCG and 5-methyl-rCGCGCG using support-aided phosphoramidite method is presented. 2'-O-Methyl guanosine derivative was separated from its 3'-O-methyl counterpart using transient 5',3'-O-silylation with 1,3-dichloro-1,1,3,3-tetraisopropyldisiloxane (Markiewicz reagent). The hexamers were obtained in a purity suitable for NMR studies.