Methylmagnesium bromide (MeMgBr, 74.0 mL, 222 mmol) was added dropwise to a tetrahydrofuran (THF, 300 mL) solution of 3-oxetanone (8 g, 111 mmol) that was cooled to 0°C. The reaction mixture was stirred at 25°C for 2 hours. After completion of the reaction, the reaction was quenched with aqueous ammonium chloride solution (NH4Cl aq). The precipitate was collected by filtration and washed with dichloromethane (DCM). The filtrate was concentrated to give 3-methyloxetan-3-ol as a light yellow oil (7.5 g, 85 mmol, 77% yield).1H NMR (400 MHz, CDCl3) δ 4.61 (d, J=6.4 Hz, 2H), 4.46 (d, J=7.2 Hz, 2H), 2.31 (s, 1H), 1.56 (s, 3H).
