A series of alternating and alternating block copolycarbonates containing the constituent groups of polysulfone was synthesized through a multi-step solution condensation method. For the regulation of block length, monodisperse oligomers were prepared by using a large excess of the bisphenols and were subsequently incorporated into the copolymer chains. Separating the unreacted bisphenols from the oligomers by dissolution/precipitation steps took advantage of solubility differences. The structures of the monomers, oligomers, and copolymers were characterized and confirmed by GPC, NMR spectroscopy, mass spectrometry, and elemental analysis. Monodispersity of the oligomers, which is critical for control over the block length in the copolymers, was confirmed by GPC and mass spectrometry. Of the two constituent groups of the polysulfone, the sulfone linkage stiffens the polycarbonate copolymer chain, while the ether linkage softens it.