2-bromo-5-methylsulfonylaniline

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of 1-bromo-4-(methylsulfonyl)-2-nitrobenzene (1.0 eq.), iron powder (3.0 eq.), and concentrated HCl (1.04 eq.) were mixed together in ethanol (0.64 M) and heated to reflux. The reaction was stirred for 24 hours, and the solvent was evaporated. The resulting residue was diluted with ethyl acetate and saturated aqueous ammonium chloride solution. The aqueous layer was extracted three times with ethyl acetate, and the combined organic layers were washed with water, brine, dried over anhydrous MgSO4, and concentrated en vacuo. The crude material was purified by triturating in 1:1 hexane/ether to give a light yellow solid. heated to reflux the solvent was evaporated The resulting residue was diluted with ethyl acetate and saturated aqueous ammonium chloride solution The aqueous layer was extracted three times with ethyl acetate the combined organic layers were washed with water, brine dried over anhydrous MgSO4 concentrated en vacuo The crude material was purified by triturating in 1:1 hexane/ether to give a light yellow solid

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of 1-bromo-4-(methylsulfonyl)-2-nitrobenzene (1.0 eq.), iron powder (3.0 eq.), and concentrated HCl (1.04 eq.) were mixed together in ethanol (0.64 M) and heated to reflux. The reaction was stirred for 24 hours, and the solvent was evaporated. The resulting residue was diluted with ethyl acetate and saturated aqueous ammonium chloride solution. The aqueous layer was extracted three times with ethyl acetate, and the combined organic layers were washed with water, brine, dried over anhydrous MgSO4, and concentrated en vacuo. The crude material was purified by triturating in 1:1 hexane/ether to give a light yellow solid. heated to reflux the solvent was evaporated The resulting residue was diluted with ethyl acetate and saturated aqueous ammonium chloride solution The aqueous layer was extracted three times with ethyl acetate the combined organic layers were washed with water, brine dried over anhydrous MgSO4 concentrated en vacuo The crude material was purified by triturating in 1:1 hexane/ether to give a light yellow solid

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of 1-bromo-4-(methylsulfonyl)-2-nitrobenzene (1.0 eq.), iron powder (3.0 eq.), and concentrated HCl (1.04 eq.) were mixed together in ethanol (0.64 M) and heated to reflux. The reaction was stirred for 24 hours, and the solvent was evaporated. The resulting residue was diluted with ethyl acetate and saturated aqueous ammonium chloride solution. The aqueous layer was extracted three times with ethyl acetate, and the combined organic layers were washed with water, brine, dried over anhydrous MgSO4, and concentrated en vacuo. The crude material was purified by triturating in 1:1 hexane/ether to give a light yellow solid. heated to reflux the solvent was evaporated The resulting residue was diluted with ethyl acetate and saturated aqueous ammonium chloride solution The aqueous layer was extracted three times with ethyl acetate the combined organic layers were washed with water, brine dried over anhydrous MgSO4 concentrated en vacuo The crude material was purified by triturating in 1:1 hexane/ether to give a light yellow solid

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of 1-bromo-4-(methylsulfonyl)-2-nitrobenzene (1.0 eq.), iron powder (3.0 eq.), and concentrated HCl (1.04 eq.) were mixed together in ethanol (0.64 M) and heated to reflux. The reaction was stirred for 24 hours, and the solvent was evaporated. The resulting residue was diluted with ethyl acetate and saturated aqueous ammonium chloride solution. The aqueous layer was extracted three times with ethyl acetate, and the combined organic layers were washed with water, brine, dried over anhydrous MgSO4, and concentrated en vacuo. The crude material was purified by triturating in 1:1 hexane/ether to give a light yellow solid. heated to reflux the solvent was evaporated The resulting residue was diluted with ethyl acetate and saturated aqueous ammonium chloride solution The aqueous layer was extracted three times with ethyl acetate the combined organic layers were washed with water, brine dried over anhydrous MgSO4 concentrated en vacuo The crude material was purified by triturating in 1:1 hexane/ether to give a light yellow solid

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of 1-bromo-4-(methylsulfonyl)-2-nitrobenzene (1.0 eq.), iron powder (3.0 eq.), and concentrated HCl (1.04 eq.) were mixed together in ethanol (0.64 M) and heated to reflux. The reaction was stirred for 24 hours, and the solvent was evaporated. The resulting residue was diluted with ethyl acetate and saturated aqueous ammonium chloride solution. The aqueous layer was extracted three times with ethyl acetate, and the combined organic layers were washed with water, brine, dried over anhydrous MgSO4, and concentrated en vacuo. The crude material was purified by triturating in 1:1 hexane/ether to give a light yellow solid. heated to reflux the solvent was evaporated The resulting residue was diluted with ethyl acetate and saturated aqueous ammonium chloride solution The aqueous layer was extracted three times with ethyl acetate the combined organic layers were washed with water, brine dried over anhydrous MgSO4 concentrated en vacuo The crude material was purified by triturating in 1:1 hexane/ether to give a light yellow solid

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of 1-bromo-4-(methylsulfonyl)-2-nitrobenzene (1.0 eq.), iron powder (3.0 eq.), and concentrated HCl (1.04 eq.) were mixed together in ethanol (0.64 M) and heated to reflux. The reaction was stirred for 24 hours, and the solvent was evaporated. The resulting residue was diluted with ethyl acetate and saturated aqueous ammonium chloride solution. The aqueous layer was extracted three times with ethyl acetate, and the combined organic layers were washed with water, brine, dried over anhydrous MgSO4, and concentrated en vacuo. The crude material was purified by triturating in 1:1 hexane/ether to give a light yellow solid. heated to reflux the solvent was evaporated The resulting residue was diluted with ethyl acetate and saturated aqueous ammonium chloride solution The aqueous layer was extracted three times with ethyl acetate the combined organic layers were washed with water, brine dried over anhydrous MgSO4 concentrated en vacuo The crude material was purified by triturating in 1:1 hexane/ether to give a light yellow solid