A very simple synthetic procedure was developed for the preparation of Ni-Sn alloy catalysts that were uti-lised for chemoselective hydrogenation of furfural, producing furfuryl alcohol almost exclusively. The mix-ture of nickel nanoparticles supported on aluminum hydroxide (R-Ni/AlOH) and a solution containing tin was treated under hydrothermal condition, producing the as prepared nickel-tin alloy supported on alumi-num hydroxide (Ni-Sn/AlOH). H2 treatment at range of temperature of 673-873 K for 1.5 h to the as pre-pared Ni-Sn/AlOH produced nanoporous Ni-Sn alloy catalysts. XRD patterns and SEM images revealed that the formation of Ni-Sn alloy of Ni3Sn and Ni3Sn2 phases and the transformation of crystalline gibbsite and bayerite into amorphous alumina were clearly observed after H2 treatment at 873 K. The formation of the Ni-Sn alloy may have played a key role in the enhancement of the chemoselectivity. © 2014 BCREC UNDIP. All rights reserved