The new acetylene-terminated monomers 1,1’-(1-methylethylidene)bis[4-(4-ethynylphenyl)methoxyl benzene and 1,3-bis[(4-ethynylphenoxy)methyl]benzene (VI) were prepared in 50% and 60% overall yield, respectively. The three-step synthesis involved : (a) a Williamson reaction between alpha,4-dibromotoluene and bisphenol A, or alpha,alpha’-dichloro-m-xylene and 4-bromophenol, giving the bromo-terminated compounds 1,1’-(1-methylethylidene)bis[4-(4-bromophenyl)methoxy]benzene or 1,3-bis[(4-bromophenoxy)methyl] benzene, respectively; (b) palladium-catalysed cross-coupling with 2-methyl-3-butyn-2-ol, affording the corresponding alkynyl tertiary alcohols from which catalyst residues were removed by treatment with diaminoethane; and (c) removal of the acetone protecting group in the presence of KOH. The low melting point of VI (102-104 degrees C) makes it suitable for catalysed cure studies.