Hydrochloric Acid → 2-methoxy-5-(trifluoromethoxy)benzoic Acid

Temperature

65 °C

To a stirred solution of 2-methoxy-5-trifluoromethoxybenzaldehyde (2.0 g, 9.09 mmol) and 50% KOH (4.1 ml) in MeOH (15 ml) at 65° C. was added dropwise hydrogen peroxide (30%, 7.4 ml) over 20 min. The reaction mixture was then stirred at 65° C. for 10 min., cooled to room temperature, acidified with 1 M HCl, and extracted with Et2O (3×40 ml). The combined organic extracts were washed with brine (35 ml), dried (Na2SO4) and the solvent removed under reduced pressure to give a pale yellow viscous oil which solidified at room temperature overnight to give the title compound (1.95 g, 91%) as a pale yellow solid.

1. temperaturecooled to room temperature
2. extractionextracted with Et2O (3×40 ml)
3. washThe combined organic extracts were washed with brine (35 ml)
4. dry with materialdried (Na2SO4)
5. customthe solvent removed under reduced pressure
6. customto give a pale yellow viscous oil which
7. waitsolidified at room temperature overnight

ORD record

ord-42d02c996db540dcaa03b8c4c3c23326

Source dataset

uspto-grants-2014_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08895313B2