The titanosilicate type CDS-1 zeolite ([Ti]CDS-1) with CDO topology can be prepared from the corresponding zeolitic layered titanosilicate [Ti]PLS-1 via dehydrative condensation of interlayers’ Q3 silanols. The precursor [Ti]PLS-1 is successfully synthesized from the mixture of an acidified kanemite, titanium tetraisopropoxide (Ti(OiPr)4), a small amount of hydrogen peroxide (H2O2), tetramethylammonium hydroxide (TMAOH) and water (H2O) under hydrothermal synthesis. The obtained samples were characterized by powder-XRD, TG–DTA, N2 adsorption, solid state NMR and UV–Vis analyses. Further oxidation reaction of terminal alkenes was examined by using H2O2 as an oxidant.