A new series of macrocyclic polyether–diester compounds containing one or two pyrazole rings (NH or N-methyl substituted) have been prepared by treating 3, 5-pyrazolyldicarbonyl chlorides with tetraethylene glycol in the presence of triethylamine. Their complexation abilities towards the shift reagent Eu (Fod) 3 have been studied by 1 H NMR in Cl 3 CD solution.