67-56-1

62089-35-4

346603-63-2

1. 2-Methyl-3-(trifluoromethyl)benzoic acid (30 g, 147 mmol) was added to a 500 mL round-bottomed flask equipped with an air condenser and a stirrer. 2. the solid was dissolved in methanol (101 mL), followed by the slow addition of sulfuric acid (8.22 mL, 154 mmol). 3. a condenser was assembled and the reaction mixture was heated to 75 °C and kept at this temperature for the reaction overnight. 4. Upon completion of the reaction, the mixture was cooled to room temperature and neutralized by the slow addition of 1N NaOH solution (~155 mL). 5. The reaction mixture was extracted with ether (3 x 300 mL), the organic layers were combined and dried over anhydrous magnesium sulfate. 6. The organic layer was concentrated under pressure to give an oil, which was further cured under vacuum to give methyl 2-methyl-3-(trifluoromethyl)benzoate as a white solid (28.25 g, 129 mmol, 88% yield). 7. The product was analyzed by 1H NMR. 7. The product was characterized by 1H NMR (400 MHz, DMSO-d6): δ 2.54 (d, J = 1.78 Hz, 3H), 3.89 (s, 3H), 7.53 (t, J = 7.83 Hz, 1H), 7.89 (d, J = 7.83 Hz, 1H), 7.97 (d, J = 7.83 Hz, 1H).