3-氯-1-(2,4-二氟苯基)丙-1-one

反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Aluminum chloride (0.3 mol) was added carefully to 1,3-difluorobenzene (0.26 mol) and the mixture was heated with vigorous stirring till 50° C. 3-Chloropropionyl chloride (0.26 mol) was added dropwise over a 15 min. period at 40° C. (cooled on ice) and the mixture was stirred at 50° C. The mixture was poured into water (250 ml), ice (250 g) and HCl (25 ml) and it was stirred for 20 min. The formed precipitate was filtered off and extracted with CH2Cl2 and water, yielding 40 g (75%) of 3-chloro-1-(2,4-di-fluorophenyl)-1-propanone (interm. 1). the mixture was heated (cooled on ice) the mixture was stirred at 50° C was stirred for 20 min The formed precipitate was filtered off extracted with CH2Cl2 and water

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a stirred mixture of aluminium (III) chloride (11.70 g, 88.0 mmol) in 1,3-difluorobenzene (21 mL) at RT was added 3-chloropropionyl chloride (4.0 mL, 41.9 mmol). The reaction mixture was stirred at 60° C. for 6 h. The mixture was cooled to RT and was poured into an ice/2M aqueous hydrochloric acid mixture (100 mL). After vigorous stirring, the mixture was extracted with DCM (2×75 ml). The combined organic extracts were dried over magnesium sulphate and concentrated in vacuo to give 8.68 g (quantitative yield) of crude title compound as an orange oil. The mixture was cooled to RT After vigorous stirring, the mixture was extracted with DCM (2×75 ml) The combined organic extracts were dried over magnesium sulphate concentrated in vacuo

反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Aluminum chloride (0.3 mol) was added carefully to 1,3-difluorobenzene (0.26 mol) and the mixture was heated with vigorous stirring till 50° C. 3-Chloropropionyl chloride (0.26 mol) was added dropwise over a 15 min. period at 40° C. (cooled on ice) and the mixture was stirred at 50° C. The mixture was poured into water (250 ml), ice (250 g) and HCl (25 ml) and it was stirred for 20 min. The formed precipitate was filtered off and extracted with CH2Cl2 and water, yielding 40 g (75%) of 3-chloro-1-(2,4-difluorophenyl)-1-propanone (interm. 1). the mixture was heated (cooled on ice) the mixture was stirred at 50° C was stirred for 20 min The formed precipitate was filtered off extracted with CH2Cl2 and water

反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Aluminum chloride (0.3 mol) was added carefully to 1,3-difluorobenzene (0.26 mol) and the mixture was heated with vigorous stirring till 50° C. 3-Chloropropionyl chloride (0.26 mol) was added dropwise over a 15 min. period at 40° C. (cooled on ice) and the mixture was stirred at 50° C. The mixture was poured into water (250 ml), ice (250 g) and HCl (25 ml) and it was stirred for 20 min. The formed precipitate was filtered off and extracted with CH2Cl2 and water, yielding 40 g (75%) of 3-chloro-1-(2,4-di-fluorophenyl)-1-propanone (interm. 1). the mixture was heated (cooled on ice) the mixture was stirred at 50° C was stirred for 20 min The formed precipitate was filtered off extracted with CH2Cl2 and water