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A series of MgAl-layered double hydroxide (MgAl-HT), the calcined form at 500 °C (MgAlOx), and the rehydrated one at 25 °C (MgAl-HT-RH) were synthesized. Physicochemical properties of the catalysts were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Surface area of the as-synthesized, calcined, and rehydrated catalysts was determined by N2 physisorption at −196 °C. CO2 temperature-programmed desorption (CO2-TPD) was applied to determine the basic sites of catalysts. The catalytic test reaction was carried out using benzaldehyde and their derivatives with nitromethane and their derivatives. The Henry products (1–15) were obtained in a very good yield using MgAl-HT-RH catalyst either by conventional method at 90 °C in liquid phase or under microwave irradiation method. The mesoporous structure and basic nature of the rehydrated solid catalyst were responsible for its superior catalytic efficiency. The robust nature was determined by using the same catalyst five times, where the product % yield was almost unchanged significantly.

MgAl-Layered Double Hydroxide Solid Base Catalysts for Henry Reaction: A Green Protocol