反应 #2821185
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06670363B1
反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 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. was then added into it over a period of 30-60 min the reaction temperature below 20° C After the addition reaction mixture was stirred at room temperature for 5-7 hours For workup, reaction mixture poured The mixture was extracted with DCE 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
来源 ID: ord-659d0e6445c143239465f19e155458d1