SIGNIFICANT ATTENTION HAS BEEN ATTRACTED TO THE UTILIZATION OF MESOPOROUS SILICA IN VARIOUS FIELDS.HOWEVER, THEIR APPLICATION IN THE ABSENCE OF SURFACE MODIFICATIONS AND FUNCTIONALIZATION IS LIMITED. BY MEANS OF MODIFICATION OF THESE MATERIALS, NEW APPLICATIONS SUCH AS MEDICAL DIAGNOSTICS, MICROELECTRONICS AND DRUG DELIVERY [1, 2] ARE REPORTED FOR THEM. MORE OVER ELECTROCHEMICAL SYNTHESES OF ORGANIC COMPOUNDS ARE GREEN METHODS THAT UTILIZE ENVIRONMENTALLY FRIENDLY SOLVENTS, WHICH IS A GREAT ADVANTAGE OF THESE METHODS [3]. IN THIS REPORT, AN ELECTROCHEMICAL SYNTHESIS METHOD WAS APPLIED FOR THE FUNCTIONALIZATION OF MESOPOROUS SILICA (MCM-41) WITH A NEW FUNCTIONAL GROUP, INCLUDING CATECHOL-BENZENSULFINIC ACID, ACHIEVE NOVEL APPLICATIONS OF THESE MATERIALS. THE MODIFICATION OF MESOPOROUS SILICA, MCM-41, USING AN ELECTROCHEMICAL METHOD HAS BEEN DEVELOPED, AND THE PROCESS WAS MONITORED BY CYCLIC VOLTAMMETERY AND SPECTROMETRIC METHODS. SULFONYLBENZENEDIOLS-FUNCTIONALIZED MCM-41 MESOPOROUS SILICA WAS CHARACTERIZED BY LOW ANGLE X-RAY DIFFRACTION, FOURIER TRANSFORM INFRARED SPECTROSCOPY, MASS SPECTROMETRY, THERMAL ANALYSIS, ELEMENTAL ANALYSIS, HIGH RESOLUTION TRANSMISSION ELECTRON MICROSCOPY, AND SURFACE AREA MEASUREMENT (SBET). THE OBTAINED RESULTS OF THIS WORK INDICATE THAT ELECTROCHEMICAL MODIFICATION OF MESOPOROUS SILICA CAN BE USED AS A NEW GREEN NOVEL TOOL FOR GRAFTING FUNCTIONAL GROUPS ONTO THESE MATERIALS IN THE ROOM TEMPERATURE.