Abstract: The syntheses of 1, 5-cyclononadiyne (3), 1, 5-~ yclodecadiyne (4), I, 5- cycloundecadiyne (9, 1, 6-cycloundecadiyne (6), 1, 6-cyclododecadiyne (7), and 1, 7- cyclododecadiyne (8) have been carried out. Diacetylenes 3 and 4 are prepared from 5- cyclononynone and 5-cyclodecynone, respectively. Compounds 5-8 are synthesized from cyclic diones by thermolysis of the corresponding bisselenadiazoles. The obtained cyclic ...