Abstract: A practical procedure is described for the total synthesis of lycophyll (16,16′-dihydroxy-lycopene; ψ,ψ-carotene-16,16′-diol), based on a C10 + C20 + C10 synthetic methodology using the commercially available materials geraniol (C10) and crocetin- dialdehyde (C20). A late-stage double Wittig olefination on crocetindialdehyde was used to form the desired lycophyll scaffold in eight linear synthetic steps, while generating a mixture of polyenic geometric isomers that could be effectively separated using HPLC. All-trans lycophyll was subsequently separated to >95% purity by semipreparative chromatography using a C30 carotenoid column.