Herein, we study adsorption and removal properties of phenazopyridine hydrochloride (PAP)from nano metal−organic framework material HKUST-1 versus bulk compound. The mechanosynthesis of HKUST-1 has been compared to its ultrasonic synthesis. It has been found that by using mechanosynthesis HKUST-1 can be obtained in a much shorter synthesis time with improved adsorption properties. Based on the obtained results for the specific surface area of products, under ultrasound-assisted methods the surface area is decreased, since the amount of the PAP adsorption decreased by this method.