Water → 5-Bromo-1,3-dichloro-2-(difluoromethoxy)benzene

To a stirred solution of 4-bromo-2,6-dichlorophenol (2.3 g) in acetonitrile (25 mL) was added potassium carbonate (1.3 g) and ethyl bromodifluoroacetate (3.8 g). The mixture was heated to reflux for 4 hours and then cooled to room temperature. The resulting mixture was poured into water (100 mL) and extracted with ethyl acetate (100 mL×1). The organic layer was washed with water and brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure to provide a residue. The residue was purified by column chromatography on silica gel eluted with ethyl acetate-hexane (1:4) to afford the title compound as yellow oil (2.4 g).

1. temperatureThe mixture was heated
2. temperatureto reflux for 4 hours
3. extractionextracted with ethyl acetate (100 mL×1)
4. washThe organic layer was washed with water and brine
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated under reduced pressure
7. customto provide a residue
8. customThe residue was purified by column chromatography on silica gel
9. washeluted with ethyl acetate-hexane (1:4)

ORD-Eintrag

ord-f3d42c03e75d4b68b9500687bcf08e21

Quelldatensatz

uspto-grants-2012_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08242283B2