The present paper shows the preparation of a highly porous periodic mesoporous organosilica (PMO) including the ionic liquid pore walls that supported with zinc ions onto PMO-IL (Zn@PMO-IL). Moreover, the material was characterized using field emission‐scanning electron microscopy, transmission electron microscopy, inductively coupled plasma, and N2 adsorption–desorption. Likewise, the catalytic activity of the Zn@PMO-IL, illustrating a highly efficient nanocatalyst for the synthesis of propargylamines through three-component A3-coupling reaction of various aldehydes, amines, and arylacetylene. The results demonstrate an eco-friendly and appealing method with high efficiency and facile work-up procedure. Furthermore, the nanocatalyst can be revived by a simple filtration process and reuse at least five successive runs without considerable reducing in its activity.
