The unusual example of click reaction occuring at both alkynyl groups present on a functionalized chain of an adenosine analogue. When the catalyst TBTA was used, only the monosubstituted product 26 was isolated. Reagents: (i) CuSO4.5H2O, sodium ascorbate, THF/H2O, rt.; (ii) CuSO4.5H2O, sodium ascorbate, TBTA, t-BuOH/H2O, rt.