Bromine → 2-Bromo-3,5-difluorophenol

A solution of 2.6 gm (20 mmol) 3,5-difluorophenol in 20 mL carbon disulfide was cooled to 0° C. and then a solution of 1.02 mL (20 mMol) bromine in 10 mL carbon disulfide was added dropwise over 30 minutes. After stirring for an additional 30 minutes, the reaction mixture was warmed to room temperature and stirred for 1.5 hours. The reaction mixture was diluted with 200 mL diethyl ether and was washed sequentially with aqueous sodium metabisulfite and saturated aqueous sodium chloride. The organic phase was then dried over sodium sulfate and concentrated under reduced pressure. The residue was vacuum distilled to provide 2.5 gm (60%) of 2-bromo-3,5-difluorophenol (b.p.=65° C. (5 mm Hg)).

1. stirringstirred for 1.5 hours
2. washwas washed sequentially with aqueous sodium metabisulfite and saturated aqueous sodium chloride
3. dry with materialThe organic phase was then dried over sodium sulfate
4. concentrationconcentrated under reduced pressure
5. distillationdistilled

ORD 기록

ord-e9581c03b5c94f1fa40f5f6e2858cee5

출처 데이터셋

uspto-grants-2006_05

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07045545B1