甲基 N-(5-氨基-2-氟苯基)氨基甲酯

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: under an atmosphere of nitrogen, compound methyl 2-fluoro-5-aminoaniline formate (72.5 mg, 0.39 mmol) was dissolved in dried DMF (5 mL), then propargyl bromide (44 μL, 0.59 mmol) and DIPEA (140 μL, 0.78 mmol) were added. The resulting solution was stirred for 6 h at 60° C., and diluted with water (10 mL) and extracted with EtOAc (10 mL×3). The combined organic phases were washed with saturated saline solution (15 mL×3), dried with anhydrous Na2SO4, concentrated and then loaded on chromatography column (PE/EtOAc=6:1-4:1) to produce a product of methyl 2-fluoro-5-(N-propargyl-imino)-aniline formate (70.1 mg, 81%); extracted with EtOAc (10 mL×3) The combined organic phases were washed with saturated saline solution (15 mL×3) dried with anhydrous Na2SO4 concentrated

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: under an atmosphere of nitrogen, compound methyl 2-fluoro-5-aminoaniline formate (72.5 mg, 0.39 mmol) was dissolved in dried DMF (5 mL), then propargyl bromide (44 μL, 0.59 mmol) and DIPEA (140 μL, 0.78 mmol) were added. The resulting solution was stirred for 6 h at 60° C., and diluted with water (10 mL) and extracted with EtOAc (10 mL×3). The combined organic phases were washed with saturated saline solution (15 mL×3), dried with anhydrous Na2SO4, concentrated and then loaded on chromatography column (PE/EtOAc=6:1-4:1) to produce a product of methyl 2-fluoro-5-(N-propargyl-imino)-aniline formate (70.1 mg, 81%); extracted with EtOAc (10 mL×3) The combined organic phases were washed with saturated saline solution (15 mL×3) dried with anhydrous Na2SO4 concentrated

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: under an atmosphere of nitrogen, compound methyl 2-fluoro-5-aminoaniline formate (72.5 mg, 0.39 mmol) was dissolved in dried DMF (5 mL), then propargyl bromide (44 μL, 0.59 mmol) and DIPEA (140 μL, 0.78 mmol) were added. The resulting solution was stirred for 6 h at 60° C., and diluted with water (10 mL) and extracted with EtOAc (10 mL×3). The combined organic phases were washed with saturated saline solution (15 mL×3), dried with anhydrous Na2SO4, concentrated and then loaded on chromatography column (PE/EtOAc=6:1-4:1) to produce a product of methyl 2-fluoro-5-(N-propargyl-imino)-aniline formate (70.1 mg, 81%); extracted with EtOAc (10 mL×3) The combined organic phases were washed with saturated saline solution (15 mL×3) dried with anhydrous Na2SO4 concentrated