2-(叔-丁基氨磺酰)乙酸

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

实验步骤: To a solution of compound 2-(N-tert-butylsulfamoyl)acetic acid (5 g, 25.6 mmol.) in dry THF (20 mL) was added HOBt (13.8 g, 102.4 mmol.) and EDCI (18.3 g, 102.4 mmol.). Then aniline (3.6 g, 38.4 mmol.) was added successively. The reaction mixture was stirred overnight at room temperature. TLC analysis showed the reaction complete. The mixture was quenched by adding water and extracted with EtOAc (30 mL×3). The combined organic layer was dried over Na2SO4, concentrated. The residue was purified by column chromatography (PE:EtOAc=2:1) to afford 2-(N-tert-butylsulfamoyl)-N-phenylacetamide (3.5 g, 51%). The mixture was quenched by adding water extracted with EtOAc (30 mL×3) The combined organic layer was dried over Na2SO4 concentrated The residue was purified by column chromatography (PE:EtOAc=2:1)

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

实验步骤: To a solution of compound 2-(N-tert-butylsulfamoyl)acetic acid (5 g, 25.6 mmol.) in dry THF (20 mL) was added HOBt (13.8 g, 102.4 mmol.) and EDCI (18.3 g, 102.4 mmol.). Then aniline (3.6 g, 38.4 mmol.) was added successively. The reaction mixture was stirred overnight at room temperature. TLC analysis showed the reaction complete. The mixture was quenched by adding water and extracted with EtOAc (30 mL×3). The combined organic layer was dried over Na2SO4, concentrated. The residue was purified by column chromatography (PE:EtOAc=2:1) to afford 2-(N-tert-butylsulfamoyl)-N-phenylacetamide (3.5 g, 51%). The mixture was quenched by adding water extracted with EtOAc (30 mL×3) The combined organic layer was dried over Na2SO4 concentrated The residue was purified by column chromatography (PE:EtOAc=2:1)

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

实验步骤: To a solution of ethyl-2-(N-tert-butylsulfamoyl)acetate (4 g, 17.9 mmol.) in 65 mL of EtOH and 13 mL of H2O at 0° C. was slowly added NaOH (3.6 g, 89.5 mmol.). The reaction was allowed to room temperature and stirred overnight. TLC analysis showed the reaction complete. The mixture was acidified to pH=5 with aq. HCl (1M). The resulting mixture was extracted with EtOAc (30 mL×3). The combined organic layer was dried over Na2SO4, concentrated to afford crude 2-(N-tert-butylsulfamoyl)acetic acid (2.4 g, 69%), which was used directly without purification. at 0° C. was allowed to room temperature The resulting mixture was extracted with EtOAc (30 mL×3) The combined organic layer was dried over Na2SO4 concentrated

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

实验步骤: To a solution of compound 2-(N-tert-butylsulfamoyl)acetic acid (5 g, 25.6 mmol.) in dry THF (20 mL) was added HOBt (13.8 g, 102.4 mmol.) and EDCI (18.3 g, 102.4 mmol.). Then aniline (3.6 g, 38.4 mmol.) was added successively. The reaction mixture was stirred overnight at room temperature. TLC analysis showed the reaction complete. The mixture was quenched by adding water and extracted with EtOAc (30 mL×3). The combined organic layer was dried over Na2SO4, concentrated. The residue was purified by column chromatography (PE:EtOAc=2:1) to afford 2-(N-tert-butylsulfamoyl)-N-phenylacetamide (3.5 g, 51%). The mixture was quenched by adding water extracted with EtOAc (30 mL×3) The combined organic layer was dried over Na2SO4 concentrated The residue was purified by column chromatography (PE:EtOAc=2:1)

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

实验步骤: To a solution of ethyl-2-(N-tert-butylsulfamoyl)acetate (4 g, 17.9 mmol.) in 65 mL of EtOH and 13 mL of H2O at 0° C. was slowly added NaOH (3.6 g, 89.5 mmol.). The reaction was allowed to room temperature and stirred overnight. TLC analysis showed the reaction complete. The mixture was acidified to pH=5 with aq. HCl (1M). The resulting mixture was extracted with EtOAc (30 mL×3). The combined organic layer was dried over Na2SO4, concentrated to afford crude 2-(N-tert-butylsulfamoyl)acetic acid (2.4 g, 69%), which was used directly without purification. at 0° C. was allowed to room temperature The resulting mixture was extracted with EtOAc (30 mL×3) The combined organic layer was dried over Na2SO4 concentrated