Sequential treatment of ω-bromoalkyl triflates with an alkynyllithium at 0° C followed by addition of a second alkynyllithium and NaI and heating the reaction mixture provides a simple one-pot access to unsymmetrical diynes in good yields. These diynes may be transformed stereoselectively into diene pheromones such as (Z, Z)-and (E, Z)-3, 13- octadecadienyl acetate.
![[(3Z,13Z)-octadeca-3,13-dienyl] acetate Structure](https://image.chemsrc.com/caspic/063/53120-27-7.png)
