Abstract: Using ¹H, ¹³C, and ¹⁵N NMR method, it was established that the formation of organic-inorganic hybrids of H₂La₂Ti₃O₁₀ with methylamine and butylamine produces intercalated alkylamino cations, while the introduction of methanol into the interlayer space of H₂La₂Ti₃O₁₀ is accompanied by the formation of covalent bonds.