ethylsulfamic acid

Conditions: temp:83.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A suspension of 93.8 parts of ethylsulfamic acid and 27 parts of paraformaldehyde in 650 parts of 1,2-dichloroethane is saturated with hydrogen chloride (72 parts) at from 10° to 15° C, whilst stirring. 0.2 part of pyridine and 142.8 parts of thionyl chloride are then added in the course of 15 minutes at 15° C. The reaction mixture is stirred for 1/2 hour at 25° C and 11/2 hour under reflux. 83.5 parts of phosphorus pentachloride are then added and the mixture is stirred for 4 hours under reflux (83° C) until the evolution of gas has ceased. On concentrating under reduced pressure, and distilling, 84 parts (58% of theory) of N-ethyl-N-chloromethylsulfamic acid chloride of boiling point 70°-75° C/0.1 mbar and nD25 = 1.4800 are obtained. The reaction mixture is stirred for 1/2 hour at 25° C 11/2 hour under reflux the mixture is stirred for 4 hours On concentrating under reduced pressure distilling

Conditions: temp:83.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A suspension of 93.8 parts of ethylsulfamic acid and 27 parts of paraformaldehyde in 650 parts of 1,2-dichloroethane is saturated with hydrogen chloride (72 parts) at from 10° to 15° C, whilst stirring. 0.2 part of pyridine and 142.8 parts of thionyl chloride are then added in the course of 15 minutes at 15° C. The reaction mixture is stirred for 1/2 hour at 25° C and 11/2 hour under reflux. 83.5 parts of phosphorus pentachloride are then added and the mixture is stirred for 4 hours under reflux (83° C) until the evolution of gas has ceased. On concentrating under reduced pressure, and distilling, 84 parts (58% of theory) of N-ethyl-N-chloromethylsulfamic acid chloride of boiling point 70°-75° C/0.1 mbar and nD25 = 1.4800 are obtained. The reaction mixture is stirred for 1/2 hour at 25° C 11/2 hour under reflux the mixture is stirred for 4 hours On concentrating under reduced pressure distilling

Conditions: temp:83.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A suspension of 93.8 parts of ethylsulfamic acid and 27 parts of paraformaldehyde in 650 parts of 1,2-dichloroethane is saturated with hydrogen chloride (72 parts) at from 10° to 15° C, whilst stirring. 0.2 part of pyridine and 142.8 parts of thionyl chloride are then added in the course of 15 minutes at 15° C. The reaction mixture is stirred for 1/2 hour at 25° C and 11/2 hour under reflux. 83.5 parts of phosphorus pentachloride are then added and the mixture is stirred for 4 hours under reflux (83° C) until the evolution of gas has ceased. On concentrating under reduced pressure, and distilling, 84 parts (58% of theory) of N-ethyl-N-chloromethylsulfamic acid chloride of boiling point 70°-75° C/0.1 mbar and nD25 = 1.4800 are obtained. The reaction mixture is stirred for 1/2 hour at 25° C 11/2 hour under reflux the mixture is stirred for 4 hours On concentrating under reduced pressure distilling