Butyrate derivatives of allyl 2-acetyl-3-(phenylamino)butanoate (1) and 1,3-dioxane derivatives of 2,6-dimethyl N-(4-methylphenyl)-1,3-dioxan-4-amine (2) and N-(3,5-diflourophenyl)-2,6-dimethyl-1,3-dioxan-4-amine (3) were synthesised. Their structures were characterized by FTIR (1) 1H NMR, 13C NMR spectroscopic techniques and single crystal X-ray diffraction. The compound (1) crystallizes in the triclinic crystal system with the space group p-1 with a = 10.0874(5) Å, b = 10.1751(5) Å, c = 14.1930(8) Å, α = 82.429(4), β = 77.482(4), γ = 80.820(4), v = 1396.77(13) Å3. The compound (2) crystallizes in the monoclinic space group P21/C with unit cell dimensions a = 9.8454(3) Å, b = 13.3032(4) Å, c = 10.1967(3) Å, α = 90, β = 114.821(2), γ = 90, v = 1212.15(6) Å3. The compound (3) crystallizes in the triclinic space group p-1 with unit cell dimensions a = 9.65630(10) Å, b = 11.2266(2) Å, c = 11.2658(2) Å, α = 83.7710(10), β = 79.1770(10), γ = 77.1290(10), v = 1166.59(3) Å3. Graphical Abstract: In the crystal packing of all the three crystal structures, the molecules are linked together by hydrogen bonds to form dimers. [Figure not available: see fulltext.] © 2013 Springer Science+Business Media New York.