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レコード

ord-c40255f429134ed694c52d15f97a4f9c

出典データセット

uspto-grants-2005_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06881733B1