Sodium Sulfate → 5-Bromo-2-(difluoromethoxy)pyridine

Participants

Reaction Steps

5-Bromopyridin-2(1H)-one (17.4 g, 100 mmol) was mixed with sodium sulfate (1.42 g, 10 mmol) and 2-(fluorosulfonyl)difluoroacetic acid (11.4 ml, 100 mmol) in acetonitrile, and stirred overnight at room temperature. Aqueous saturated sodium hydrogencarbonate solution was added to the reaction solution, and the solvent was concentrated under reduced pressure. The residue was dissolved in diethyl ether, washed with saturated saline, the organic layer was dried with sodium sulfate, and the solvent was evaporated off under reduced pressure. The residue was purified through silica gel column chromatography (eluate: ethyl acetate/hexane=20/80 to 50/50) to obtain the entitled compound (18.75 g, 84%) as a pale yellow oily substance.

Provenance & Evidence