Hydrochloric Acid → 6-Bromo-3-(difluoromethoxy)-2-methoxyphenol

Temperatur

50 °C

To a stirring solution of 1-bromo-4-(difluoromethoxy)-3-methoxy-2-(methoxymethoxy)benzene (1 g, 3.19 mmol) in methanol (15 mL) was added concentrated hydrochloride (2 mL) and the reaction mixture was heated to 50° C. for 1 h. The reaction mixture was cooled to RT, concentrated under reduced pressure and the obtained residue was basified with sodium bicarbonate solution and extracted with dichloromethane (3×). The combined dichloromethane layers were washed with brine, dried over sodium sulphate and concentrated under reduced pressure to afford the title compound as a solid (800 mg, 93%).

1. temperatureThe reaction mixture was cooled to RT
2. concentrationconcentrated under reduced pressure
3. extractionextracted with dichloromethane (3×)
4. washThe combined dichloromethane layers were washed with brine
5. dry with materialdried over sodium sulphate
6. concentrationconcentrated under reduced pressure

ORD-Eintrag

ord-52dc51a924b54c9d8c3c20a2acf80d1c

Quelldatensatz

uspto-grants-2015_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09051290B2