Hydrogen Peroxide → HCID 23159686, compound

Participants

Reaction Steps

16.2 g (104.4 mmol) of an aqueous 30% hydrogen peroxide was dropped to 13.8 g (52.2 mmol) of the crude 2-trifluoromethyl-3-fluoro-4-ethoxyphenyl boronic acid obtained in the third step dissolved in 100 ml of THF, and further stirred at a room temperature for 2 hours. The solution was poured into 300 ml of an aqueous saturated sodium hydrogen sulfite solution and extracted with 200 ml of ethyl acetate. The organic layer was washed with 300 ml of an aqueous saturated sodium hydrogen sulfite solution, with 300 ml of water, and then with 200 ml an aqueous saturated sodium chloride solution successively and, after drying over anhydrous magnesium sulfate, concentrated under a reduced pressure. The residue was purified by distillation and further recrystallized twice from a heptane/ethanol mixed solvent to obtain 5.67 g of pure 2-trifluoromethyl-3-fluoro-4-ethoxyphenol.

Provenance & Evidence