Hydrochloric Acid → 4-(2,2,2-Trifluoroethoxy)benzoic acid

Temperatur

65 °C

To a stirred solution of 50% w/v KOH (1.2 ml) and 4-(2,2,2-trifluoroethoxy)-benzaldehyde (0.6 g, 2.94 mmol) in MeOH (5 ml) at 65° C. was added dropwise over 20 min aqueous hydrogen peroxide (30 wt. % in water, 2.4 ml). On completion of the addition the reaction mixture was heated at 65° C. for a further 10 min. On cooling to room temperature, the reaction mixture was acidified with 1 M HCl and extracted with Et2O (3×30 ml). The combined organic extracts were washed with brine (20 ml), dried (Na2SO4) and the solvent removed under reduced pressure to give the title compound (0.59 g, 91%) as a pale yellow solid which was used without further purification.

1. customat 65° C.
2. additionOn completion of the addition the reaction mixture
3. temperatureOn cooling to room temperature
4. extractionextracted with Et2O (3×30 ml)
5. washThe combined organic extracts were washed with brine (20 ml)
6. dry with materialdried (Na2SO4)
7. customthe solvent removed under reduced pressure

ORD-Eintrag

ord-2f2e71168b0443d89330b97e317e4e09

Quelldatensatz

uspto-grants-2014_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08895313B2