[Y(O2CNBu2)3], has been prepared by extraction of the Y3+ ions from aqueous solution into heptane by the NHBu2/CO2 system. Exhaustive hydrolysis of [Y(O2CNBu2)3] produced the yttrium carbonate [Y2(CO3)3⋅n H2O] (n=2–3), that was converted to Y2O3 by thermal treatment at 550°C for 12h. The exhaustive hydrolysis of [Y(O2CNBu2)3] and [Al(OBu)3] (Y/Al molar ratio=3/5) carried out at room temperature yielded an intermediate mixed carbonate, that, upon heating at 950°C for 12h, was converted to Y3Al5O12. The exhaustive hydrolysis of [Y(O2CNBu2)3] and [Al(OBu)3] was repeated in the presence of [Nd(O2CNBu2)3] (Nd/Y molar ratio=0.07;(Nd+Y)/Al molar ratio=3:5). The neodymium doped garnet Nd:Y3Al5O12 was obtained, through the intermediate formation of a mixed hydroxo-carbonate. For comparison, the neodymium doped garnet was prepared also starting from N,N-dialkylcarbamato complexes of all three metals, [Y(O2CNBu2)3], [Nd(O2CNBu2)3] and [Al2(O2CNiPr2)6] (Nd/Y molar ratio=0.07;(Nd+Y)/Al molar ratio=3:5). Also in this case the intermediate mixed hydroxo-carbonate, after heating at 950°C for 12h, evolved to Nd:Y3Al5O12.FTIR, XRD, SEM, TGA measurements were used for the characterization of the obtained materials. Preliminary studies of the photoluminescent emission properties were carried out on Nd:Y3Al5O12. Photoluminescence dynamics have been investigated by means of femtosecond laser pulses and nanosecond temporal resolution up to the millisecond range after excitation. All the luminescence traces have shown a decay time of the order 200 microseconds indicating its potential as a laser medium for infrared emission at 1064nm.