反应 #2990131
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07951810B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of tert-butyl[2-(aminomethyl)benzyl]carbamate (0.2 g, 0.93 mmol) and triethylamine (260 μL, 1.9 mmol) in DCM (10 mL) was added AC2O (0.285 g, 0.00279 mol) dropwise and the reaction stirred for 2 h at r.t. The reaction was concentrated, the residue dissolved in EtOAc (20 mL) then washed with saturated aq NaHCO3 (2×10 mL). The organic layer was dried (Na2SO4) and concentrated to give the crude product (0.25 g, 90%). To a solution of this in DCM (5 mL) was added 2 mL of 4M HCl/dioxane and the solution was stirred for 1 h. The reaction was concentrated to give the title compound (0.16 g, 95%) which was used without further purification. The reaction was concentrated the residue dissolved in EtOAc (20 mL) then washed with saturated aq NaHCO3 (2×10 mL) The organic layer was dried (Na2SO4) concentrated to give the crude product (0.25 g, 90%) the solution was stirred for 1 h The reaction was concentrated
来源 ID: ord-86db6f52bab34846b670dd2bcc4b7f07