N-(3-chloropropyl)sulfamoyl chloride

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

Procedure: To sulfuryl chloride (5 g, 30.05 mmol) in acetonitrile (30 mL), was added 3-chloropropyl amine hydrochloride (486 mg, 5.00 mmol). The reaction mixture was allowed to react over 18 hr at 75-80° C. After the completion of the reaction, the resultant was concentrated under reduced pressure, extracted with ether and then kept under vacuum for a long time to remove remained sulfuryl chloride, giving 3-chloropropylsulfamoyl chloride that was used without further purification. to react over 18 hr at 75-80° C After the completion of the reaction the resultant was concentrated under reduced pressure extracted with ether to remove

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

Procedure: To sulfuryl chloride (5 g, 30.05 mmol) in acetonitrile (30 mL), was added 3-chloropropyl amine hydrochloride (486 mg, 5.00 mmol). The reaction mixture was allowed to react at 80° C., evaporated and then extracted with diethyl ether and H2O, followed by evaporation of the organic layer under vacuum, to give 3-chloropropylsulfamoyl chloride that was used without further purification. to react at 80° C. evaporated extracted with diethyl ether and H2O followed by evaporation of the organic layer under vacuum