Three amphiphilic compounds having a triple bond at one end and a related compound have been synthesised. DSC studies show that three of them are mesogens. Multilayer films of these compounds have been formed by thermal evaporation in vacuo and by the Langmuir-Blodgett method. Attempts to polymerise and cross-link these films by the agency of UV light in a nitrogen atmosphere have been made. This process was carried out both on films in the liquid crystal state and on the films in the two dimensional crystalline state. Both untreated and polymerised films were characterised by X-ray diffraction and by polarising microscopy.