Hydrochloric Acid → HCID 14983824, compound

Temperature

0 °C

Into the solution of 1,3-Difluorobenzene in 1,2-dicholoroethane (DCE) was added anhydrous aluminium chloride (1.2 mol eqnt.) at 25-30° C. and stirred for 30 minutes. The reaction mixture was then cooled to 0° C. and (±)2-chloropropionyl chloride (1.1 molar equivalent), diluted in DCE, was then added into it over a period of 30-60 min keeping the reaction temperature below 20° C. After the addition was over, reaction mixture was stirred at room temperature for 5-7 hours. For workup, reaction mixture was diluted with DCE and poured into chilled aq. hydrochloric acid solution (5%). The mixture was extracted with DCE and the combined organic layer was washed with 5% aq. sodium bicarbonate solution and water. The solvent was evaporated off under reduced pressure to afford an oil.

1. additionwas then added into it over a period of 30-60 min
2. customthe reaction temperature below 20° C
3. additionAfter the addition
4. customreaction mixture
5. stirringwas stirred at room temperature for 5-7 hours
6. customFor workup, reaction mixture
7. additionpoured
8. extractionThe mixture was extracted with DCE
9. washthe combined organic layer was washed with 5% aq. sodium bicarbonate solution and water
10. customThe solvent was evaporated off under reduced pressure
11. customto afford an oil

ORD record

ord-659d0e6445c143239465f19e155458d1

Source dataset

uspto-grants-2003_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06670363B1