反应 #1600677
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06673790B1
反应条件: temp:-60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 26.3 g of 4-chlorophenylamine in 150 ml of dichloromethane and 35 ml of triethylamine are added, at −60° C., to 22 g of 2-oxopropionyl chloride (prepared according to Synthesis, 1975, 163-164 from 2-oxopropionic acid and 1,1-dichlorodimethyl ether) in 350 ml of dichloromethane. The reaction mixture is stirred at −60° C. for 2 hours and then 200 ml of a 0.15N aqueous hydrochloric acid solution and 500 ml of dichloromethane are added at −30° C. The organic phase is extracted, washed with a 0.25N aqueous hydrochloric acid solution and dried over sodium sulphate. The solvents are evaporated under reduced pressure and the residue obtained is crystallized from dichloromethane; The organic phase is extracted washed with a 0.25N aqueous hydrochloric acid solution dried over sodium sulphate The solvents are evaporated under reduced pressure the residue obtained is crystallized from dichloromethane
来源 ID: ord-e665b7dfb5434b6596ef75489748249a