Several studies have shown the interest of organo-modified 2:1 phyllosilicates as fillers for polymers to enhance thermal, mechanical or barrier properties. Montmorillonite were particularly investigated whereas only a few studies deals with talc like structures. Organic-inorganic talc like hybrids (TLH) can be prepared by a process based on sol-gel chemistry which enables the formation of the materials under mild conditions in a one-step method. In this case, the organic groups are linked directly to the inorganic framework by covalent bonds whereas, in the case of montmorillonite only low energy bonds are obtained between the silicate layers and the organic moieties or surfactants. This method allows the production of a variety of TLH based compound with different organic moities bringing specific properties. In this study, the sol-gel synthesis of organic-inorganic talc like hybrids having the following chemical formula: Mg3(RSi)4O8(OH)2 (where R stands for the organic part) starting from diethylphosphatoethyltriethoxysilane (SiP) and an ethanolic solution of magnesium nitrate hexahydrate was optimised. It was shown that by using short aging times (5 min to 1 day) and low volume of solvent at room temperature, it is possible to form a range of lamellar structures as confirmed by XRD. FTIR, TGA 13C, 31P and 29Si NMR analysis confirmed the integrity of organic moieties in the TLH structure and enables gathering information on the degree of polycondensation of the silicon species