1-chloro-N-propan-2-ylmethanesulfonamide

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

実験手順: A 32.3 g (0.32 mol) sample of triethylamine was added dropwise to a cooled (0° C.) solution of 50 g (0.29 mol) N-isopropyl chloromethanesulfonamide and 70 g (0.29 mol) 1,1,2,2-tetrachloroethylsulfenyl chloride. After the addition was completed, the reaction was stirred at ambient temperature for 30 minutes and then under reflux for 3 hours. The reaction mixture was then cooled, washed with water, dried over magnesium sulfate and evaporated under reduced pressure to give the N-isopropyl-N-(trichlorovinylthio)-chloromethanesulfonamide product, which after crystallization from pet. ether melted at 71°-73° C. The product is reported as Compound 1. After the addition under reflux for 3 hours The reaction mixture was then cooled washed with water dried over magnesium sulfate evaporated under reduced pressure

反応条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A 11.8 g (0.2 mol) sample of isopropylamine was added dropwise to a cooled (-60° C.) solution of 19.3 g (0.1 mol) chloromethanesulfonyl bromide in 200 ml dichloromethane. The reaction was then allowed to warm to about 25° C. and stirred about 16 hours. The reaction mixture was then filtered, washed with water, dried over magnesium sulfate and evaporated to give crude N-isopropyl chloromethanesulfonamide. The reaction mixture was then filtered washed with water dried over magnesium sulfate evaporated

反応条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A 11.8 g (0.2 mol) sample of isopropylamine was added dropwise to a cooled (-60° C.) solution of 19.3 g (0.1 mol) chloromethanesulfonyl bromide in 200 ml dichloromethane. The reaction was then allowed to warm to about 25° C. and stirred about 16 hours. The reaction mixture was then filtered, washed with water, dried over magnesium sulfate and evaporated to give crude N-isopropyl chloromethanesulfonamide. The reaction mixture was then filtered washed with water dried over magnesium sulfate evaporated

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

実験手順: A 32.3 g (0.32 mol) sample of triethylamine was added dropwise to a cooled (0° C.) solution of 50 g (0.29 mol) N-isopropyl chloromethanesulfonamide and 70 g (0.29 mol) 1,1,2,2-tetrachloroethylsulfenyl chloride. After the addition was completed, the reaction was stirred at ambient temperature for 30 minutes and then under reflux for 3 hours. The reaction mixture was then cooled, washed with water, dried over magnesium sulfate and evaporated under reduced pressure to give the N-isopropyl-N-(trichlorovinylthio)-chloromethanesulfonamide product, which after crystallization from pet. ether melted at 71°-73° C. The product is reported as Compound 1. After the addition under reflux for 3 hours The reaction mixture was then cooled washed with water dried over magnesium sulfate evaporated under reduced pressure

反応条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A 11.8 g (0.2 mol) sample of isopropylamine was added dropwise to a cooled (-60° C.) solution of 19.3 g (0.1 mol) chloromethanesulfonyl bromide in 200 ml dichloromethane. The reaction was then allowed to warm to about 25° C. and stirred about 16 hours. The reaction mixture was then filtered, washed with water, dried over magnesium sulfate and evaporated to give crude N-isopropyl chloromethanesulfonamide. The reaction mixture was then filtered washed with water dried over magnesium sulfate evaporated