(2,6-dichlorophenyl)methanesulfonamide

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:170.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The 2,6-dichlorobenzylsulfonamide (8 g, 33.47 mmol) was added to potassium carbonate (4.62 g, 33.47 mmol), copper powder (560 milligram (hereinafter “mg”)) and N,N-dimethylaniline (10 ml) in a round bottom flask. The reaction mixture was stirred at 170° C. for about 4 hours. then was cooled to room temperature and partitioned between ethyl acetate and 10% aqueous HCl. The combined organic phase was dried and concentrated. Chromatography of the residue on silica gel (30% Ethyl acetate/Hexane) gave desired product (4 g, 59%). EI-MS m/z 204.5 (M+). then was cooled to room temperature partitioned between ethyl acetate and 10% aqueous HCl The combined organic phase was dried concentrated

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

実験手順: The 2,6-dichlorobenzylsulfonylchloride (27 g, 103.6 mmol) in ammonium hydroxide (270 ml) was stirred at room temperature for about 3 hours. On acidification with cooled concentrated hydrochloric acid a precipitate separated and was filtered to give desired product (16 g, 64%) EI-MS m/z 239 (M−). separated was filtered

反応条件: temp:170.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The 2,6-dichlorobenzylsulfonamide (8 g, 33.47 mmol) was added to potassium carbonate (4.62 g, 33.47 mmol), copper powder (560 milligrams (hereinafter“mg”)) and N,N-dimethylaniline (10 ml) in flask. The reaction mixture was stirred at 170° C. for 4 hours, then it was cooled to room temperature and partitioned between ethyl acetate and 10% aqueous HCl. The combined organic phase was dried and concentrated. Chromatography of the residue on silica gel (30% Ethyl acetate/Hexane) gave desired product (4 g, 59%). MS(EI) m/e 204.5 (M+). it was cooled to room temperature partitioned between ethyl acetate and 10% aqueous HCl The combined organic phase was dried concentrated

反応条件: temp:170.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The 2,6-dichlorobenzylsulfonamide (8 g, 33.47 mmol) was added to potassium carbonate (4.62 g, 33.47 mmol), copper powder (560 milligrams (hereinafter“mg”)) and N,N-dimethylaniline (10 ml) in flask. The reaction mixture was stirred at 170° C. for 4 hours, then it was cooled to room temperature and partitioned between ethyl acetate and 10% aqueous HCl. The combined organic phase was dried and concentrated. Chromatography of the residue on silica gel (30% Ethyl acetate/Hexane) gave desired product (4 g, 59%). MS(EI) m/e 204.5 (M+). it was cooled to room temperature partitioned between ethyl acetate and 10% aqueous HCl The combined organic phase was dried concentrated

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

実験手順: The 2,6-dichlorobenzylsulfonylchloride (27 g, 103.6 mmol) in ammonium hydroxide (270 ml) was stirred at room temperature for 3 hours. On acidification with cooled concentrated hydrochloric acid a precipitate separated and was filtered to give desired product (16 g, 64%) MS(EI) m/e 239 (M−). separated was filtered

反応条件: temp:170.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The 2,6-dichlorobenzylsulfonamide (8 g, 33.47 mmol) was added to potassium carbonate (4.62 g, 33.47 mmol), copper powder (560 milligram (hereinafter “mg”)) and N,N-dimethylaniline (10 ml) in a round bottom flask. The reaction mixture was stirred at 170° C. for about 4 hours. then was cooled to room temperature and partitioned between ethyl acetate and 10% aqueous HCl. The combined organic phase was dried and concentrated. Chromatography of the residue on silica gel (30% Ethyl acetate/Hexane) gave desired product (4 g, 59%). EI-MS m/z 204.5 (M+). then was cooled to room temperature partitioned between ethyl acetate and 10% aqueous HCl The combined organic phase was dried concentrated

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

実験手順: The 2,6-dichlorobenzylsulfonylchloride (27 g, 103.6 mmol) in ammonium hydroxide (270 ml) was stirred at room temperature for about 3 hours. On acidification with cooled concentrated hydrochloric acid a precipitate separated and was filtered to give desired product (16 g, 64%) EI-MS m/z 239 (M−). separated was filtered

反応条件: temp:170.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The 2,6-dichlorobenzylsulfonamide (8 g, 33.47 mmol) was added to potassium carbonate (4.62 g, 33.47 mmol), copper powder (560 milligram (hereinafter “mg”)) and N,N-dimethylaniline (10 ml) in a round bottom flask. The reaction mixture was stirred at 170° C. for about 4 hours. then was cooled to room temperature and partitioned between ethyl acetate and 10% aqueous HCl. The combined organic phase was dried and concentrated. Chromatography of the residue on silica gel (30% Ethyl acetate/Hexane) gave desired product (4 g, 59%). EI-MS m/z 204.5 (M+). then was cooled to room temperature partitioned between ethyl acetate and 10% aqueous HCl The combined organic phase was dried concentrated

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:170.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The 2,6-dichlorobenzylsulfonamide (8 g, 33.47 mmol) was added to potassium carbonate (4.62 g, 33.47 mmol), copper powder (560 milligrams (hereinafter“mg”)) and N,N-dimethylaniline (10 ml) in flask. The reaction mixture was stirred at 170° C. for 4 hours, then it was cooled to room temperature and partitioned between ethyl acetate and 10% aqueous HCl. The combined organic phase was dried and concentrated. Chromatography of the residue on silica gel (30% Ethyl acetate/Hexane) gave desired product (4 g, 59%). MS(EI) m/e 204.5 (M+). it was cooled to room temperature partitioned between ethyl acetate and 10% aqueous HCl The combined organic phase was dried concentrated

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

実験手順: The 2,6-dichlorobenzylsulfonylchloride (27 g, 103.6 mmol) in ammonium hydroxide (270 ml) was stirred at room temperature for 3 hours. On acidification with cooled concentrated hydrochloric acid a precipitate separated and was filtered to give desired product (16 g, 64%) MS(EI) m/e 239 (M−). separated was filtered