反应 #3758538
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08093424B2
反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of 6,8-difluoro-3,4-dihydro-2H-naphthalen-1-one (1.0 gram, 5.5 moles) and potassium thiophenolate (0.81 gram, 5.5 mmole) in 4 mL DMSO was heated at 50° C. for 0.5 hour. The mixture was diluted with 30 mL 0.1N hydrochloric acid and then it was extracted with 50 mL diethyl ether. The organic phase was washed with water, dried (magnesium sulfate) and concentrated under reduced pressure. 8-Fluoro-6-phenylsulfanyl-3,4-dihydro-2H-naphthalen-1-one was obtained by recrystallization of the residue from ethyl acetate/hexane, 0.871 gram (58%), m.p. 112-113° C., M+H=273. it was extracted with 50 mL diethyl ether The organic phase was washed with water dried (magnesium sulfate) concentrated under reduced pressure
来源 ID: ord-42171410f7da43f7aac848a784776060