反应 #1970404
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07713979B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Dissolve 4-oxo-4-(2-oxo-oxazolidin-3-yl)-butyraldehyde (7.35 g, 42.96 mmol) in DCE (400 mL). Add 8-methyl-1,4-dioxa-spiro[4.5]dec-8-ylamine (7.36 g, 42.96 mmol), and acetic acid (2.58 g, 42.96 mmol) at room temperature under nitrogen. Stir the solution for one hour and then add sodium triacetoxyborohydride (18.21 g, 85.92 mmol). Stir the reaction mixture for over night and then add water (400 mL). Extract the aqueous layer with dichloromethane (3×400 mL). Combine the organic layers and dry with Na2SO4, filter, concentrate and purify by flash column chromatography (silica gel, 20-50% of EtOAc-Hexane) to give 0.92 g (9.0%) of 1-(8-Methyl-1,4-dioxa-spiro[4.5]dec-8-yl)-pyrrolidin-2-one as a colorless oil. at room temperature Stir the reaction mixture for over night Extract the aqueous layer with dichloromethane (3×400 mL) Combine the organic layers and dry with Na2SO4 filter concentrate purify by flash column chromatography (silica gel, 20-50% of EtOAc-Hexane)
来源 ID: ord-5e21d6d609904d63879f8b9f433e961a