3-Hydroxy-2,2-dimethylpropionic acid (15.00 g, 127.0 mmol) was dissolved in methanol (200 mL), concentrated sulfuric acid (13.5 g, 254 mmol) was added, and the reaction was stirred under reflux conditions for 16 hours. After completion of the reaction, the reaction mixture was concentrated under vacuum, diluted with ethyl acetate (100 mL) and washed sequentially with water (2 x 50 mL), saturated aqueous sodium bicarbonate solution (50 mL), water (50 mL) and brine (50 mL). The organic phase was dried with anhydrous sodium sulfate and the organic solvent was subsequently removed under vacuum to afford methyl 3-hydroxy-2,2-dimethylpropionate (6.4 g, 57.2% yield) as a colorless liquid.1H NMR (400 MHz, DMSO-d6) δ: 3.71 (s, 3H), 3.56 (s, 2H), 2.05-2.04 (m, 1H), 1.19 ( s, 6H).
