Iodine in liquid ammoriia has been found to be an effective reagent for the direct iodination of monosubstituted acetylenes. Phenyl, tolyl and vinyl acetylenes react with iodine in ammonia at-34'giving almost theoretical yields of the corresponding iodoacetylene. Ethyl, butyl, amyl and heptyl acetylenes react slowly with ammonia solutions of iodine at-34". At 25" 1545% yields of the iodoacetylenes are obtained.