The non-phosgene carbonylation of 1,6-hexamethylenediamine (HDA) with alkyl carbamates using Y(NO3)(3)center dot 6H(2)O as a catalyst and the influence of reaction variables on the yields of dialkyl hexamethylenedicarbamate (HDC) were studied. At 453 K and in the presence of 5wt.% Y(NO3)(3)center dot 6H(2)O, nearly 100% HDA conversion and 85% dibutyl hexamethylenedicarbamate (BHDC) isolated yield could be achieved when butyl carbamate (BC) was employed as a carbonyl source. During reaction, an induction period was observed, but it almost disappeared by pretreating the catalyst with n-butanol. The FT-IR, X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) characterizations of the catalyst showed that some transformation occurred when the catalyst was pretreated with n-butanol or employed during reaction, i.e., part decomposition of Y(NO3)(3) to Y2O3, conversion from crystal to amorphous state, changes occurring in chemical state of the active species, as well as some subtle interactions between the catalyst and n-butanol. All these observed changes might be the reason resulting in activation of the catalyst. (C) 2008 Published by Elsevier B.V.