Nanostructured N doped TiO 2 efficient stable catalyst for Kabachnik-Fields reaction under microwave irradiation.

Herein, we report nitrogen-doped TiO 2 (N-TiO 2 ) solid-acid nanocatalysts with heterogeneous structure employed for the solvent-free synthesis of α-aminophosphonates through Kabachnik-Fields reaction. N-TiO 2 were synthesized by direct amination using triethylamine as a source of nitrogen at low temperature and optimized by varying the volume ratios of TiCl 4 , methanol, water, and triethylamine, under identical conditions. An X-ray diffraction (XRD) study showed the formation of a rutile phase and the crystalline size is 10 nm. The nanostructural features of N-TiO 2 were examined by HR-TEM analysis, which showed they had rod-like morphology with a diameter of ∼7 to 10 nm. Diffuse reflectance spectra show the extended absorbance in the visible region with a narrowing in the band gap of 2.85 eV, and the high resolution XPS spectrum of the N 1s region confirmed successful doping of N in the TiO 2 lattice. More significantly, we found that as-synthesized N-TiO 2 showed significantly higher catalytic activity than commercially available TiO 2 for the synthesis of a novel series of α-amino phosphonates via Kabachnik-Fields reaction under microwave irradiation conditions. The improved catalytic activity is due to the presence of strong and Bronsted acid sites on a porous nanorod surface. This work signifies N-TiO 2 is an efficient stable catalyst for the synthesis of α-aminophosphonate derivatives.