The synthesis of a nido-carboranyl congener of misonidazole, 1-(3'-nido-carboranyl-2'-hydroxy)propyl-2-nitroimidazole, has been carried out. Alternative methods of preparations were conducted to optimize the chemical yield, with a five step synthesis giving an overall yield (from 1,2-carborane) of 36%. A diastereomeric pair of nido-carboranyl compounds was obtained. The diastereomeric nido-carboranyl misonidazole congeners were (radio)iodinated to yield (> 90%) a mixture of diastereomeric compounds in which the iodine had bonded to a boron atom on the nido-carborane moiety. These compounds will be investigated for their application to boron neutron capture therapy (BNCT) and hypoxia imaging of cancer.