Hydrogen Peroxide → HCID 23159686, compound

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.

1. customobtained in the third step
2. extractionextracted with 200 ml of ethyl acetate
3. washThe organic layer was washed with 300 ml of an aqueous saturated sodium hydrogen sulfite solution, with 300 ml of water
4. dry with materialwith 200 ml an aqueous saturated sodium chloride solution successively and, after drying over anhydrous magnesium sulfate
5. concentrationconcentrated under a reduced pressure
6. distillationThe residue was purified by distillation
7. customfurther recrystallized twice from a heptane/ethanol mixed solvent

ORD record

ord-c3ef6fd8d07d471bb8a247964c1fd86b

Source dataset

uspto-grants-2010_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07838087B2