N,N-Dimethylmethanesulfonamide was obtained by acylation of dimethylamine with methanesulfonyl chloride.

Triethylamine (1.01 g, 10 mmol) was added to a solution of dimethylamine (10 mmol) dissolved in 20 mL of CH2Cl2 at -20 °C. Then, methanesulfonyl chloride (15 mmol) was slowly added at -20 °C. After stirring for 6 hours from -20 °C to room temperature, an aqueous solution of NH4Cl (3 mL) was added to the reaction mixture. The solution was extracted with CH2Cl2 (3 × 50 mL), and the combined organic phases were washed with H2O (3 × 10 mL) and brine, dried over MgSO4, filtered, and concentrated under vacuum.
The residue was purified by silica gel chromatography using hexane-ether (10:1) as the eluent to give sulfonamide.