反应 #1083643
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06451734B1
反应条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: At 0° C., 36.3 g (0.46 mol) of pyridine and then within 2 hours a solution of 42.5 g (0.19 mol) of 2,3-dichlorophenylacetyl chloride in 100 ml of dichloromethane were added dropwise to a solution of 28.8 g (0.20 mol) of Meldrum's acid in 200 ml of dichloromethane. The mixture was then stirred for 12 hours at about 20° C. and subsequently stirred into 100 ml of 10% strength hydrochloric acid. The organic phase was then separated off and the aqueous phase was extracted two more times with dichloromethane. Finally, the combined extracts were dried over magnesium sulfate and concentrated. The residue was dissolved in 300 ml of methanol and heated under reflux until the formation of gas had ceased. The mixture was then concentrated. Yield: quantitative. The organic phase was then separated off the aqueous phase was extracted two more times with dichloromethane Finally, the combined extracts were dried over magnesium sulfate concentrated The residue was dissolved in 300 ml of methanol heated under reflux until the formation of gas The mixture was then concentrated
来源 ID: ord-ac6e4d747f374406a9ef82f548e476e1