An iron (III) carboxylate Metal Organic Framework isostructural with MIL-100(Fe) was synthesized through a mechanochemical route. The material, rapidly obtained by liquid-assisted grinding at room temperature, was characterized by X-ray powder diffraction, infrared spectroscopy, scanning electron microscopy, thermal gravimetry, nitrogen physisorption and adsorption microcalorimetry of ammonia. For comparison, the features of a commercial iron trimesate produced via electrochemical route were investigated as well. The ball-milled sample showed better crystallinity, associated with good thermal stability, higher surface area and pore volume. The adsorption performance of both the ball-milled and commercial samples for the ambient-temperature removal of 4,6-dimethyldibenzothiophene (4,6-DMDBT) from 4,6-DMDBT)/n-heptane solutions simulating a diesel fuel was also investigated. The maximum adsorption capacity for the ball-milled sample resulted twice as big as that for the commercial one. An interpretation of the different adsorption behavior is proposed.