The reaction between the alkyne, N- (5-Benzyloxy-2-pentynyl) phthalimide and decaborane (14) in the presence of dimethyl sulfide resulted in the isolation of 1-C 6 H 4 (CO) 2 NCH 2 -2-C 6 H 5 CH 2 OCH 2 CH 2 -1, 2-C 2 B 1 0 H 1 0 (5) , 1-methylphthalimido-2-ethylbenzyl ether-o-carborane, in moderate yield. Compound 5 was characterized by single crystal X-ray diffraction study. Compound 5 crystallizes in the P1 space group, a=10.5328 (5) 9, b=11.9209 (6) 9, c=10.3451 (3) 9, α=110.492 (3) o , β=102.868 (3) o , γ=87.279 (2) o , Z=2, D c a l c =1.226 g\cm 3 , R=0.0491 for 3521 reflections with F>4.0σ. Deprotection of the ether linkage of 5 results in the formation of 1-C 6 H 4 (CO) 2 NCH 2 -2-HOCH 2 CH 2 -1, 2-C 2 B 1 0 H 1 0 (6) , 1-methylphthalimido-2-ethylalcohol-o-carborane. The transformation is accomplished by hydrogenation of (5) over a Pd\C catalyst and resulted in the efficient conversion of (5) into (6) (83% yield) . Experimental details and analytical data leading to the identification of the reported compounds is provided.