反应 #1486980
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09150556B2
反应条件: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a mixture of 1-fluoro-2-nitrobenzene (450 □L, 4.3 mmol) and (1-amino-cyclohexyl)-acetic acid methyl ester (880 mg, 5.2 mmol) in DMF (5 mL) was added DIPEA (1.0 mL, 5.7 mmol). The mixture was heated at 90° C. for 16 hours. The reaction mixture was allowed to cool to room temperature, diluted with EtOAc (50 mL) and washed with H2O (50 mL×3). The organic layer was dried over sodium sulfate and concentrated. The resulting residue was purified by CombiFlash with 20% EtOAc in Hexane as the eluent to afford the desired [1-(2-nitro-phenylamino)-cyclohexyl]-acetic acid methyl ester (230 mg, 19%). to cool to room temperature washed with H2O (50 mL×3) The organic layer was dried over sodium sulfate concentrated The resulting residue was purified by CombiFlash with 20% EtOAc in Hexane as the eluent
来源 ID: ord-28d730dab3384e5c97f84463c2c7d5e1