sodium;2-methoxy-2-oxoethanesulfonate

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

実験手順: The sodium methoxycarbonylmethylsulfonate salt was added in small portions to a stirred solution of 840 ml (9.14 mols) phosphorus oxychloride. The resulting mixture was then heated at 80°-100° C. for about 5 hours and allowed to cool overnight. The reaction mixture was filtered, the filtered solid was washed with dichloromethane and the filtrate distilled under reduced pressure to remove the dichloromethane and excess phosphorus oxychloride. The resulting oil residue was distilled through a short Vigreaux column to give 226.8 g (65.7% yield) of methoxycarbonylmethylsulfonyl chloride, as a yellow oil, b.p. 79°-80° C. (0.5 mm Hg). The resulting mixture was then heated at 80°-100° C. for about 5 hours to cool overnight The reaction mixture was filtered the filtered solid was washed with dichloromethane the filtrate distilled under reduced pressure to remove the dichloromethane and excess phosphorus oxychloride The resulting oil residue was distilled through a short Vigreaux column

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

実験手順: A slurry of 217 g (2 mols) methyl chloroactate and 252 g (2 mols) sodium sulfite in 500 ml water was stirred and heated under reflux for about 2 hours. The resulting solution was allowed to stand at about 25° C. for 56 hours and then evaporated under reduced pressure to give solid residue. The residue was washed with acetone and dried under vacuum at 80°-90° C. to give crude sodium methoxycarbonylmethylsulfonate salt. heated under reflux for about 2 hours evaporated under reduced pressure to give solid residue The residue was washed with acetone dried under vacuum at 80°-90° C.

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

実験手順: A slurry of 217 g (2 mols) methyl chloroactate and 252 g (2 mols) sodium sulfite in 500 ml water was stirred and heated under reflux for about 2 hours. The resulting solution was allowed to stand at about 25° C. for 56 hours and then evaporated under reduced pressure to give solid residue. The residue was washed with acetone and dried under vacuum at 80°-90° C. to give crude sodium methoxycarbonylmethylsulfonate salt. heated under reflux for about 2 hours evaporated under reduced pressure to give solid residue The residue was washed with acetone dried under vacuum at 80°-90° C.

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

実験手順: The sodium methoxycarbonylmethylsulfonate salt was added in small portions to a stirred solution of 840 ml (9.14 mols) phosphorus oxychloride. The resulting mixture was then heated at 80°-100° C. for about 5 hours and allowed to cool overnight. The reaction mixture was filtered, the filtered solid was washed with dichloromethane and the filtrate distilled under reduced pressure to remove the dichloromethane and excess phosphorus oxychloride. The resulting oil residue was distilled through a short Vigreaux column to give 226.8 g (65.7% yield) of methoxycarbonylmethylsulfonyl chloride, as a yellow oil, b.p. 79°-80° C. (0.5 mm Hg). The resulting mixture was then heated at 80°-100° C. for about 5 hours to cool overnight The reaction mixture was filtered the filtered solid was washed with dichloromethane the filtrate distilled under reduced pressure to remove the dichloromethane and excess phosphorus oxychloride The resulting oil residue was distilled through a short Vigreaux column

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

実験手順: A slurry of 217 g (2 mols) methyl chloroacetate and 252 g (2 mols) sodium sulfite in 500 ml water was stirred and heated under reflux for about 2 hours. The resulting solution was allowed to stand at about 25° C. for 56 hours and then evaporated under reduced pressure to give solid residue. The residue was washed with acetone and dried under vacuum at 80°-90° C. to give crude sodium methoxycarbonylmethylsulfonate salt. heated under reflux for about 2 hours evaporated under reduced pressure to give solid residue The residue was washed with acetone dried under vacuum at 80°-90° C.

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

実験手順: A slurry of 217 g (2 mols) methyl chloroacetate and 252 g (2 mols) sodium sulfite in 500 ml water was stirred and heated under reflux for about 2 hours. The resulting solution was allowed to stand at about 25° C. for 56 hours and then evaporated under reduced pressure to give solid residue. The residue was washed with acetone and dried under vacuum at 80°-90° C. to give crude sodium methoxycarbonylmethylsulfonate salt. heated under reflux for about 2 hours evaporated under reduced pressure to give solid residue The residue was washed with acetone dried under vacuum at 80°-90° C.

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

実験手順: The sodium methoxycarbonylmethylsulfonate salt was added in small portions to a stirred solution of 840 ml (9.14 mols) phosphorus oxychloride. The resulting mixture was then heated at 80°-100° C for about 5 hours and allowed to cool overnight. The reaction mixture was filtered, the filtered solid was washed with dichloromethane and the filtrate distilled under reduced pressure to remove the dichloromethane and excess phosphorus oxychloride. The resulting oil residue was distilled through a short Vigreaux column to give 226.8 g (65.7% yield) of methoxycarbonylmethylsulfonyl chloride, as a yellow oil, b.p. 79°-80° C. (0.5 mm Hg). The resulting mixture was then heated at 80°-100° C for about 5 hours to cool overnight The reaction mixture was filtered the filtered solid was washed with dichloromethane the filtrate distilled under reduced pressure to remove the dichloromethane and excess phosphorus oxychloride The resulting oil residue was distilled through a short Vigreaux column

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

実験手順: A slurry of 217 g (2 mols) methyl chloroacetate and 252 g (2 mols) sodium sulfite in 500 ml water was stirred and heated under reflux for about 2 hours. The resulting solution was allowed to stand at about 25° C for 56 hours and then evaporated under reduced pressure to give solid residue. The residue was washed with acetone and dried under vacuum at 80°-90° C to give crude sodium methoxycarbonylmethylsulfonate salt. heated under reflux for about 2 hours evaporated under reduced pressure to give solid residue The residue was washed with acetone dried under vacuum at 80°-90° C

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

実験手順: The sodium methoxycarbonylmethylsulfonate salt was added in small portions to a stirred solution of 840 ml (9.14 mols) phosphorus oxychloride. The resulting mixture was then heated at 80°-100° C. for about 5 hours and allowed to cool overnight. The reaction mixture was filtered, the filtered solid was washed with dichloromethane and the filtrate distilled under reduced pressure to remove the dichloromethane and excess phosphorus oxychloride. The resulting oil residue was distilled through a short Vigreaux column to give 226.8 g (65.7% yield) of methoxycarbonylmethylsulfonyl chloride, as a yellow oil, b.p. 79°-80° C. (0.5 mm Hg). The resulting mixture was then heated at 80°-100° C. for about 5 hours to cool overnight The reaction mixture was filtered the filtered solid was washed with dichloromethane the filtrate distilled under reduced pressure to remove the dichloromethane and excess phosphorus oxychloride The resulting oil residue was distilled through a short Vigreaux column

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

実験手順: A slurry of 217 g (2 mols) methyl chloroactate and 252 g (2 mols) sodium sulfite in 500 ml water was stirred and heated under reflux for about 2 hours. The resulting solution was allowed to stand at about 25° C. for 56 hours and then evaporated under reduced pressure to give solid residue. The residue was washed with acetone and dried under vacuum at 80°-90° C. to give crude sodium methoxycarbonylmethylsulfonate salt. heated under reflux for about 2 hours evaporated under reduced pressure to give solid residue The residue was washed with acetone dried under vacuum at 80°-90° C.

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

実験手順: The sodium methoxycarbonylmethylsulfonate salt was added in small portions to a stirred solution of 840 ml (9.14 mols) phosphorus oxychloride. The resulting mixture was then heated at 80°-100° C. for about 5 hours and allowed to cool overnight. The reaction mixture was filtered, the filtered solid was washed with dichloromethane and the filtrate distilled under reduced pressure to remove the dichloromethane and excess phosphorus oxychloride. The resulting oil residue was distilled through a short Vigreaux column to give 226.8 g (65.7% yield) of methoxycarbonylmethylsulfonyl chloride, as a yellow oil, b.p. 79°-80° C. (0.5 mm Hg). The resulting mixture was then heated at 80°-100° C. for about 5 hours to cool overnight The reaction mixture was filtered the filtered solid was washed with dichloromethane the filtrate distilled under reduced pressure to remove the dichloromethane and excess phosphorus oxychloride The resulting oil residue was distilled through a short Vigreaux column

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

実験手順: A slurry of 217 g (2 mols) methyl chloroacetate and 252 g (2 mols) sodium sulfite in 500 ml water was stirred and heated under reflux for about 2 hours. The resulting solution was allowed to stand at about 25° C. for 56 hours and then evaporated under reduced pressure to give solid residue. The residue was washed with acetone and dried under vacuum at 80°-90° C. to give crude sodium methoxycarbonylmethylsulfonate salt. heated under reflux for about 2 hours evaporated under reduced pressure to give solid residue The residue was washed with acetone dried under vacuum at 80°-90° C.