反应 #3250359
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08969568B2
反应条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 100 mg 6.1 and 70 mg of (S)-5-(aminomethyl)oxazolidine-2-one (2.19) (50%) were dissolved in dimethylacetamide. 0.175 mL (1.01 mmol) of diisopropylethylamine was added and the mixture was heated at 70° C. for 30 minutes and overnight at ambient temperature. The mixture was diluted with 20 mL dichloromethane and 20 mL water. The phases were separated and the water phase extracted with additional 10 mL dichloromethane. The combined organic phases were concentrated and the product purified via chromatography (SiO2:dichloromethane→dichloromethane/methanol 90:10). The product was recrystallized from ethyl acetate and methyl-tert-butylether. The phases were separated the water phase extracted with additional 10 mL dichloromethane The combined organic phases were concentrated the product purified via chromatography (SiO2:dichloromethane→dichloromethane/methanol 90:10) The product was recrystallized from ethyl acetate and methyl-tert-butylether
来源 ID: ord-65ecf8d02c80451bb34e48f97e755346