Hydrochloric Acid → 2-Chloro-1-(3,4-difluorophenyl)ethanone

Temperatur

60 °C

1,2-Difluorobenzene (150 g) and aluminium chloride (156 g) were charged in a round bottom flask. The reaction mixture is heated to about 60° C. followed by slow addition of chloroacetyl chloride (105 mL) over a period of 1 hour at the same temperature. The reaction mixture was stirred for another 3 hours followed by cooling to about 10° C. The reaction mass was poured into precooled water (1500 mL) followed by addition of hydrochloric acid (36%, 225 mL) at the same temperature and stirring. To this mixture ethyl acetate (750 mL) was charged and layers were separated. The aqueous layer is extracted with ethyl acetate (750 mL). The organic layers were combined and washed with water (750 mL) followed by complete evaporation of organic layer under vacuum at 50-55° C. The residue obtained is cooled to 25-35° C. followed by purification with column chromatography using 0-5% ethyl acetate in petroleum ether to afford the title compound in about 70% yield having HPLC purity of 99.51%.

1. temperatureby cooling to about 10° C
2. stirringstirring
3. customlayers were separated
4. extractionThe aqueous layer is extracted with ethyl acetate (750 mL)
5. washwashed with water (750 mL)
6. customfollowed by complete evaporation of organic layer under vacuum at 50-55° C
7. customThe residue obtained
8. temperatureis cooled to 25-35° C.
9. customfollowed by purification with column chromatography

ORD-Eintrag

ord-7d4365a7957542038a842d9eff747f40

Quelldatensatz

uspto-grants-2016_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09233966B2