General procedure: To a solution of 2-(methylamino)ethanol (500 mg, 0.53 mL, 6.66 mmol) in dichloromethane (20 mL) was added di-tert-butyl dicarbonate (1.48 g, 6.79 mmol), and the reaction was stirred at room temperature for 1 hour. After completion of the reaction, the reaction mixture was extracted with saturated aqueous sodium chloride solution and dichloromethane. The organic layers were combined, dried with anhydrous magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure to give N-BOC-N-methylaminoethanol (colorless oil, quantitative yield). The product was characterized as follows: 1H NMR (200 MHz, CDCl3) δ 3.74 (q, J = 10.5, 5.2 Hz, 2H), 3.25 (t, J = 5.2 Hz, 2H), 2.91 (s, 3H), 1.45 (s, 9H); mass spectra m/z (relative intensities) 144 (20), 102 (24), 57 (70), 44 (100).
