反应 #3546539
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07863293B2
反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of 4-aminobutyraldehyde dimethyl acetal (2.73 g, 20.5 mmol) in THF (50 mL) was added 1,1′-carbonyldiimidazole (3.39 g, 20.9 mmol) and the resultant mixture was stirred at room temperature for 45 minutes. The mixture was concentrated under reduced pressure and the residue was dissolved in DMF (50 mL) and treated with DIPEA (18 mL, 103 mmol) and benzyloxyamine hydrochloride (10.2 g, 64.0 mmol). The mixture was heated at 60° C. overnight then concentrated under reduced pressure. The residue was dissolved in EtOAc (200 mL) and the solution was washed with brine (5×25 mL), dried (MgSO4), and concentrated. Purification of the crude material by column chromatography on silica gel (4:1 hexanes-EtOAc followed by 100% EtOAc) provided 4.29 g (73%) of 3-(4,4-dimethoxy-butyl)-1-(benzyloxy)-urea as a yellow oil. The mixture was concentrated under reduced pressure the residue was dissolved in DMF (50 mL) then concentrated under reduced pressure The residue was dissolved in EtOAc (200 mL) the solution was washed with brine (5×25 mL) dried (MgSO4) concentrated Purification of the crude material by column chromatography on silica gel (4:1 hexanes-EtOAc followed by 100% EtOAc)
来源 ID: ord-b91478e2789d474299a4248f03a3680c