Reference of 346603-63-2, The chemical industry reduces the impact on the environment during synthesis 346603-63-2, name is Methyl 2-methyl-3-(trifluoromethyl)benzoate, I believe this compound will play a more active role in future production and life.
To a 1 L round bottom flask equipped with a stir bar, nitrogen lines, and pressure equalizing addition funnel, was added lithium aluminum deuteride (LAD) (12 g, 286 mmol). The solid material was taken up in anhydrous tetrahydrofuran (THF) (268 ml) and the resulting suspension placed under a nitrogen atmosphere and the temperature lowered to 0 0C. The addition funnel was then charged with a solution of methyl 2-methyl-3- (trifluoromethyl)benzoate (27 g, 124 mmol) in anhydrous tetrahydrofuran (THF) (107 ml), and the substrate was slowly added, drop-wise, to the LAD suspension over approximately 30 minutes. Upon complete addition, the funnel was removed and the inert atmosphere maintained. The reaction temperature was allowed to warm naturally to ambient over 2 hours with vigorous stirring. The reaction was then quenched with a modified Fieser and Fieser workup (adjusting by multiplying normal lithium aluminum hydride reduction workup amount by .8564) by sequential addition of the following: 10.277 mL water, 10.277 mL of 15 wt % NaOH (aq.) solution, and 30.83 mL water. The resulting mixture was stirred at room temperature for 1 hour to allow the precipitate to form and was then filtered, followed by concentration of the solution, in vacuo, to afford a gel. The gel was suspended in dichloromethane and transferred to a 100 mL round bottom flask. The material was concentrated to a gel and then subjected to high vacuum to afford [2-methyl- 3-(trifluoromethyl)phenyl]methanol-d2 (21.883 g, 114 mmol, 92 % yield) as a white solid 1H NMR (400 MHz, DMSO-J6) delta ppm 2.33 (d, J=I.52 Hz, 3H) 5.26 (s, IH) 7.37 (t, J=7.71 Hz, IH) 7.57 (d, J=7.83 Hz, IH) 7.67 (d, J=7.83 Hz, IH).
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, Methyl 2-methyl-3-(trifluoromethyl)benzoate, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; GLAXOSMITHKLINE LLC; LIN, Hong; LUENGO, Juan, I.; RIVERO, Ralph, A.; SCHULZ, Mark, James; XIE, Ren; ZENG, Jin; WO2010/135504; (2010); A1;,
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