1-(benzenesulfonyl)-3-bromopropan-2-one

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a suspension of 50 g (0.180 mole) finely ground 1-bromo-3-phenylsulfonylpropan-2-one (the product of Example 10) in 125 ml methylene chloride cooled to about 0°-5° C., 36.8 g (0.54 mole) imidazole in 300 ml methylene chloride were added dropwise. The reaction mixture was maintained at 0°-5° C. for one hour, allowed to warm to room temperature and was stirred overnight. The methylene chloride was removed in vacuo at room temperature. The resulting oil was partitioned with 200 ml water and 200 ml ethyl acetate. The aqueous phase was extracted with ethyl acetate (four times 125 ml). The combined ethyl acetate extracts were treated with decolorizing charcoal, dried, filtered and concentrated. The precipitate which formed was triturated with methanol-isopropyl alcohol yielding 17.9 g of the above-identified product, as an off-white solid, melting point 137°-140° C. cooled to about 0°-5° C. The reaction mixture was maintained at 0°-5° C. for one hour The methylene chloride was removed in vacuo at room temperature The resulting oil was partitioned with 200 ml water and 200 ml ethyl acetate The aqueous phase was extracted with ethyl acetate (four times 125 ml) The combined ethyl acetate extracts were treated with decolorizing charcoal dried filtered concentrated The precipitate which formed was triturated with methanol-isopropyl alcohol yielding 17.9 g of the above-identified product, as an off-white solid, melting point 137°-140° C.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a stirred suspension of 100.0 g (0.504 mole) phenylsulfonylacetone in 500 ml carbon tetrachloride, 80 g [25.7 ml (0.5 mole)] bromine dissolved in 75 g carbon tetrachloride were added dropwise. The reaction mixture was stirred at ambient temperature overnight. The reaction mixture was filtered, and the precipitate was washed with hexane to give 139.8 g of the above-identified product. were added dropwise The reaction mixture was filtered the precipitate was washed with hexane

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a stirred suspension of 100.0 g (0.504 mole) phenylsulfonylacetone in 500 ml carbon tetrachloride, 80 g [25.7 ml (0.5 mole)] bromine dissolved in 75 g carbon tetrachloride were added dropwise. The reaction mixture was stirred at ambient temperature overnight. The reaction mixture was filtered, and the precipitate was washed with hexane to give 139.8 g of the above-identified product. were added dropwise The reaction mixture was filtered the precipitate was washed with hexane

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a suspension of 50 g (0.180 mole) finely ground 1-bromo-3-phenylsulfonylpropan-2-one (the product of Example 10) in 125 ml methylene chloride cooled to about 0°-5° C., 36.8 g (0.54 mole) imidazole in 300 ml methylene chloride were added dropwise. The reaction mixture was maintained at 0°-5° C. for one hour, allowed to warm to room temperature and was stirred overnight. The methylene chloride was removed in vacuo at room temperature. The resulting oil was partitioned with 200 ml water and 200 ml ethyl acetate. The aqueous phase was extracted with ethyl acetate (four times 125 ml). The combined ethyl acetate extracts were treated with decolorizing charcoal, dried, filtered and concentrated. The precipitate which formed was triturated with methanol-isopropyl alcohol yielding 17.9 g of the above-identified product, as an off-white solid, melting point 137°-140° C. cooled to about 0°-5° C. The reaction mixture was maintained at 0°-5° C. for one hour The methylene chloride was removed in vacuo at room temperature The resulting oil was partitioned with 200 ml water and 200 ml ethyl acetate The aqueous phase was extracted with ethyl acetate (four times 125 ml) The combined ethyl acetate extracts were treated with decolorizing charcoal dried filtered concentrated The precipitate which formed was triturated with methanol-isopropyl alcohol yielding 17.9 g of the above-identified product, as an off-white solid, melting point 137°-140° C.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a stirred suspension of 100.0 g (0.504 mole) phenylsulfonylacetone in 500 ml carbon tetrachloride, 80 g [25.7 ml (0.5 mole)] bromine dissolved in 75 g carbon tetrachloride were added dropwise. The reaction mixture was stirred at ambient temperature overnight. The reaction mixture was filtered, and the precipitate was washed with hexane to give 139.8 g of the above-identified product. were added dropwise The reaction mixture was filtered the precipitate was washed with hexane