N,N-二乙基-3-氨基苯磺酰胺

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

实验步骤: The N,N-diethyl-3-(nitro)benzenesulfonamide (3.9 g) was dissolved in methanol (60 ml) and, after an addition of conc. hydrochloric acid (10 ml), reduced iron (4.2 g) was added and the mixture was stirred at room temperature for 2 hours. After filtration, methanol was evaporated under a reduced pressure and the residue was made basic with an addition of 4 N sodium hydroxide. The iron oxide precipitated was separated by filtration, washed with methylene chloride (50 ml). Also the filtrate was extracted with methylene (50 ml ×2) and combined with the methylene chloride washing, followed by drying over anhydrous sodium sulfate Evaporation of the solvent gave N,N-diethyl-3-(amino)benzenesulfonamide (3.0 g) (m.p. 82°-84° C.). was added After filtration, methanol was evaporated under a reduced pressure the residue was made basic with an addition of 4 N sodium hydroxide The iron oxide precipitated was separated by filtration washed with methylene chloride (50 ml) Also the filtrate was extracted with methylene (50 ml ×2) by drying over anhydrous sodium sulfate Evaporation of the solvent

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

实验步骤: The N,N-diethyl-3-(nitro)benzenesulfonamide (3.9 g) was dissolved in methanol (60 ml) and, after an addition of conc. hydrochloric acid (10 ml), reduced iron (4.2 g) was added and the mixture was stirred at room temperature for 2 hours. After filtration, methanol was evaporated under a reduced pressure and the residue was made basic with an addition of 4N sodium hydroxide. The iron oxide precipitated was separated by filtration, washed with methylene chloride (50 ml). Also the filtrate was extracted with methylene (50 ml×2) and combined with the methylene chloride washing, followed by drying over anhydrous sodium sulfate. Evaporation of the solvent gave N,N-diethyl-3-(amino)benzenesulfonamide (3.0 g) (m.p. 82°-84° C.). was added After filtration, methanol was evaporated under a reduced pressure the residue was made basic with an addition of 4N sodium hydroxide The iron oxide precipitated was separated by filtration washed with methylene chloride (50 ml) Also the filtrate was extracted with methylene (50 ml×2) by drying over anhydrous sodium sulfate Evaporation of the solvent