A series of bis(alkyl)thioether compounds utilising biphenyl as the backbone of the type 2,2′-bis(alkylthio)-1,1′-biphenyl have been prepared with yields of 32-70%. The six benzyl derivatives all displayed an AB quartet for the CH2 hydrogens within their 1 H NMR spectra due to restricted rotation within the molecule. Where the alkyl group was changed to neopentyl the CH2 protons became equivalent giving rise to a singlet within the 1 H NMR spectrum. The compounds have been characterised principally using multinuclear NMR spectroscopy and single crystal X-ray diffraction.