[3-(carbamimidoylsulfanyl)propyl]dimethylamine dihydrochloride

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A stirred mixture of 1-chloro-3-(dimethylamino) propane hydrochloride (305.7 g), thiourea (150 g) and ethanol (1530 ml) was heated under reflux for 24 hours then cooled to ambient temperature. Ethyl acetate was added until a faint opalescence was observed, then the mixture was stored at 4° C. for 72 hours. The resulting solid was collected by filtration, washed with ethyl acetate, and dried in vacuo at 40° C. to give S-[3-(dimethylamino)propyl]isothiourea dihydrochloride as a white solid (403 g), m.p. 155°-157° C. was heated under reflux for 24 hours The resulting solid was collected by filtration washed with ethyl acetate dried in vacuo at 40° C.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A stirred mixture of 1-chloro-3-(dimethylamino) propane hydrochloride (305.7 g), thiourea (150 g) and ethanol (1530 ml) was heated under reflux for 24 hours then cooled to ambient temperature. Ethyl acetate was added until a faint opalescence was observed, then the mixture was stored at 4° C. for 72 hours. The resulting solid was collected by filtration, washed with ethyl acetate, and dried in vacuo at 40° C. to give S-[3-(dimethylamino)propyl]isothiourea dihydrochloride as a white solid (403 g), m.p. 155°-157° C. was heated under reflux for 24 hours The resulting solid was collected by filtration washed with ethyl acetate dried in vacuo at 40° C.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 1-chloro-3-(dimethylamino)propane hydrochloride (200 g), thiourea (98.1 g) and ethanol (11) was stirred and heated under reflux for 25 hours. The solution was cooled to ambient temperature and ethyl acetate added until permanent opalescence was obtained. The mixture was stored at 4° C. overnight then filtered to give S-[3-(dimethylamino)propyl]isothiourea dihydrochloride as a colourless solid. (283 g), m.p. 155°-159° C. heated under reflux for 25 hours was obtained then filtered

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 1-chloro-3-(dimethylamino)propane hydrochloride (200 g), thiourea (98.1 g) and ethanol (11) was stirred and heated under reflux for 25 hours. The solution was cooled to ambient temperature and ethyl acetate added until permanent opalescence was obtained. The mixture was stored at 4° C. overnight then filtered to give S-[3-(dimethylamino)propyl]isothiourea dihydrochloride as a colourless solid. (283 g), m.p. 155°-159° C. heated under reflux for 25 hours was obtained then filtered

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A stirred mixture of 1-chloro-3-(dimethylamino) propane hydrochloride (305.7 g), thiourea (150 g) and ethanol (1530 ml) was heated under reflux for 24 hours then cooled to ambient temperature. Ethyl acetate was added until a faint opalescence was observed, then the mixture was stored at 4° C. for 72 hours. The resulting solid was collected by filtration, washed with ethyl acetate, and dried in vacuo at 40° C. to give S-[3-(dimethylamino)propyl]isothiourea dihydrochloride as a white solid (403 g), m.p. 155°-157° C. was heated under reflux for 24 hours The resulting solid was collected by filtration washed with ethyl acetate dried in vacuo at 40° C.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 1-chloro-3-(dimethylamino)propane hydrochloride (200 g), thiourea (98.1 g) and ethanol (11) was stirred and heated under reflux for 25 hours. The solution was cooled to ambient temperature and ethyl acetate added until permanent opalescence was obtained. The mixture was stored at 4° C. overnight then filtered to give S-[3-(dimethylamino)propyl]isothiourea dihydrochloride as a colourless solid. (283 g), m.p. 155°-159° C. heated under reflux for 25 hours was obtained then filtered

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Equimolar quantities of thiourea and 3-(dimethylamino)-1-chloropropane hydrochloride and a little ethanol are heated together at 140° for 3 hours, and the cooled mixture is recrystallised from methanol/isopropanol to give the title product. the cooled mixture is recrystallised from methanol/isopropanol

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 3-(Dimethylamino)-1-chloropropane hydrochloride (79 g) in ethanol (300 ml) was added over a period of 5 mins to a mixture of thiourea (38 g) in ethanol (500 ml). The resultant mixture was boiled under reflux and ethanol (100 ml) was removed by distillation. Further quantities of 3-(dimethylamino)-1-chloropropane hydrochloride (8 g and 4 g) were added after 30 hrs and 54 hrs. refluxing. After the mixture had boiled under reflux for a total of 78 hours the solvent was removed by evaporation to give a moist solid which was filtered off and recrystallised from methanol/isopropanol to give the title product (92.9 g, 79%) m.p. 160.5°-161.5°. under reflux ethanol (100 ml) was removed by distillation Further quantities of 3-(dimethylamino)-1-chloropropane hydrochloride (8 g and 4 g) were added after 30 hrs and 54 hrs refluxing under reflux for a total of 78 hours the solvent was removed by evaporation to give a moist solid which was filtered off recrystallised from methanol/isopropanol

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A stirred mixture of 1-chloro-3-(dimethylamino) propane hydrochloride (305.7 g), thiourea (150 g) and ethanol (1530 ml) was heated under reflux for 24 hours then cooled to ambient temperature. Ethyl acetate was added until a faint opalescence was observed, then the mixture was stored at 4° C. for 72 hours. The resulting solid was collected by filtration, washed with ethyl acetate, and dried in vacuo at 40° C. to give S-[3-(dimethylamino)propyl]isothiourea dihydrochloride as a white solid (403 g), m.p. 155°-157° C. was heated under reflux for 24 hours The resulting solid was collected by filtration washed with ethyl acetate dried in vacuo at 40° C.

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 1-chloro-3-(dimethylamino)propane hydrochloride (200 g), thiourea (98.1 g) and ethanol (11) was stirred and heated under reflux for 25 hours. The solution was cooled to ambient temperature and ethyl acetate added until permanent opalescence was obtained. The mixture was stored at 4° C. overnight then filtered to give S-[3-(dimethylamino)propyl]isothiourea dihydrochloride as a colourless solid. (283 g), m.p. 155°-159° C. heated under reflux for 25 hours was obtained then filtered