Hydrochloric Acid → 1-(4-Bromo-2,5-difluorophenyl)ethan-1-one

Temperature

60 °C

Acetyl chloride (17 ml) is slowly dropped into a stirred mixture of 1-bromo-2,5-difluorobenzene (30 g) and aluminium trichloride (53 g) heated at 60° C. and kept under argon. The reaction mixture is then stirred 90 minutes at 95° C. The mixture is cooled at 40° C. and carefully poured into crushed ice (400 g) and concentrated hydrochloric acid (35 ml). The resulting mixture is stirred a few minutes and then extracted with ethyl ether (2×250 ml). The ethereal solution is washed to neutral with brine, dried over sodium sulfate and the solvent is evaporated. The distillation of the oily residue gives 4'-bromo-2 ',5'-difluoroacetophenone (21.2 g) b.p. (0.05 mm)=60° C.

1. temperatureThe mixture is cooled at 40° C.
2. additioncarefully poured
3. stirringThe resulting mixture is stirred a few minutes
4. extractionextracted with ethyl ether (2×250 ml)
5. washThe ethereal solution is washed to neutral with brine
6. dry with materialdried over sodium sulfate
7. customthe solvent is evaporated
8. distillationThe distillation of the oily residue

ORD record

ord-198b147a0184444fb062f6bd53d235b0

Source dataset

uspto-grants-1998_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05786350