Water → 2-(Difluoromethoxy)-4-fluoro-1-nitrobenzene

Temperatur

100 °C

To a solution of 5-fluoro-2-nitrophenol (3.1 g, 20 mmol) in DMF (40 mL), potassium carbonate (4.2 g, 30 mmol) and chlorodifluoroacetic acid methyl ester (3.2 mL, 30 mmol) were successively added at room temperature. Subsequently, the temperature of the mixture was raised to 100° C., and the mixture was stirred for 2 hours. The mixture was cooled to room temperature, and water (100 mL) was added to the reaction mixture, followed by extraction with diethyl ether (200 mL) once. The organic layer was successively washed with water (100 mL) and a saturated aqueous sodium chloride solution (100 mL), and after it was dried with sodium sulfate, the solvent was distilled off under reduced pressure. The obtained residue was purified by silica gel column chromatography to give the title compound (3.1 g, yield: 75%).

1. temperatureThe mixture was cooled to room temperature
2. extractionfollowed by extraction with diethyl ether (200 mL) once
3. washThe organic layer was successively washed with water (100 mL)
4. dry with materiala saturated aqueous sodium chloride solution (100 mL), and after it was dried with sodium sulfate
5. distillationthe solvent was distilled off under reduced pressure
6. customThe obtained residue was purified by silica gel column chromatography

ORD-Eintrag

ord-967b46609911433aadfc12495ed11469

Quelldatensatz

uspto-grants-2014_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08642640B2