Cu(I)-catalyzed Glaser-Hey-type cross coupling of 9ethynylnoscapine with terminal alkynes has been described that enables synthesis of unsymmetrical noscapine 1,3-diynes in very good yields in the presence of base and amines as ligands. The symmetrical dimer of 9-ethynylnoscapine was also isolated as by-product. Outcome of these couplings critically depends on the choice of ligands and base as well as employed reaction conditions. The synthesized 1,3-diyne analogues were evaluated for their antiproliferative activity. . Percentage growth against NCI 60 subpanel tumor cell lines in vitro at 10 μM concentration of the noscapinoids 7 g, 7 i and 8.