Potassium Hydroxide → 4-Bromo-2-chloro-1-(difluoromethoxy)benzene

温度

80 °C

A solution of 4-bromo-2-chlorophenol (830 mg) and a 30% potassium hydroxide solution (16 mL) in acetonitrile (16 mL) was cooled to −78° C. 2-Chloro-2,2-difluoroacetophenone (2.95 mL) was added and the mixture was stirred at 80° C. for 40 hours. The reaction solution was cooled to room temperature and extracted with diethyl ether. The organic layer was washed with water and brine, dried over anhydrous magnesium sulfate and filtered. The solvent was then evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=10:1→10:1) to give 4-bromo-2-chloro-1-(difluoromethoxy)benzene as a colorless oil (533 mg, 52%).

1. temperatureThe reaction solution was cooled to room temperature
2. extractionextracted with diethyl ether
3. washThe organic layer was washed with water and brine
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationfiltered
6. customThe solvent was then evaporated under reduced pressure
7. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=10:1→10:1)

ORDレコード

ord-1c82bc8a453045e1bd8067176806964e

出典データセット

uspto-grants-2014_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08822503B2