4-氯-N,N-二甲基丁-1-胺;盐酸盐

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-4-(dimethylamino)-butane hydrochloride (115 g), thiourea (51.9 g) and ethanol (500 ml) was heated under reflux for 24 hours then allowed to stand at 4° C. for 24 hours. The resulting solid was collected by filtration, washed with ether, and dried in vacuo at ambient temperature for 24 hours to give S-[4-(dimethylamino)butyl]isothiourea dihydrochloride as an off-white solid (140 g), m.p. 179°-182° C. was heated under reflux for 24 hours The resulting solid was collected by filtration washed with ether dried in vacuo at ambient temperature for 24 hours

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-4-(dimethylamino)-butane hydrochloride (115 g), thiourea (51.9 g) and ethanol (500 ml) was heated under reflux for 24 hours then allowed to stand at 4° C. for 24 hours. The resulting solid was collected by filtration, washed with ether, and dried in vacuo at ambient temperature for 24 hours to give S-[4-(dimethylamino)butyl]isothiourea dihydrochloride as an off-white solid (140 g), m.p. 179°-182° C. was heated under reflux for 24 hours The resulting solid was collected by filtration washed with ether dried in vacuo at ambient temperature for 24 hours

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

实验步骤: 4-(Dimethylamino)butanol (88.5g) was added dropwise at 0° C. over 2 hours to stirred thionyl chloride (93.4 g) then the mixture was stirred at ambient temperature for 1 hour and poured into ethanol (500 ml). The stirred solution was heated under reflux for 10 minutes, then the solvent was removed in vacuo. The solid residue crystallised from ethanol as a white solid which was collected by filtration, washed with ethanol, and dried in vacuo at ambient temperature for 24 hours to give 1-chloro-4-(dimethylamino)butane hydrochloride as a white solid (115 g), m.p. 100°-105° C. The stirred solution was heated under reflux for 10 minutes the solvent was removed in vacuo The solid residue crystallised from ethanol as a white solid which was collected by filtration washed with ethanol dried in vacuo at ambient temperature for 24 hours

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

实验步骤: 4-(Dimethylamino)butanol (88.5g) was added dropwise at 0° C. over 2 hours to stirred thionyl chloride (93.4 g) then the mixture was stirred at ambient temperature for 1 hour and poured into ethanol (500 ml). The stirred solution was heated under reflux for 10 minutes, then the solvent was removed in vacuo. The solid residue crystallised from ethanol as a white solid which was collected by filtration, washed with ethanol, and dried in vacuo at ambient temperature for 24 hours to give 1-chloro-4-(dimethylamino)butane hydrochloride as a white solid (115 g), m.p. 100°-105° C. The stirred solution was heated under reflux for 10 minutes the solvent was removed in vacuo The solid residue crystallised from ethanol as a white solid which was collected by filtration washed with ethanol dried in vacuo at ambient temperature for 24 hours

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-4-(dimethylamino)-butane hydrochloride (115 g), thiourea (51.9 g) and ethanol (500 ml) was heated under reflux for 24 hours then allowed to stand at 4° C. for 24 hours. The resulting solid was collected by filtration, washed with ether, and dried in vacuo at ambient temperature for 24 hours to give S-[4-(dimethylamino)butyl]isothiourea dihydrochloride as an off-white solid (140 g), m.p. 179°-182° C. was heated under reflux for 24 hours The resulting solid was collected by filtration washed with ether dried in vacuo at ambient temperature for 24 hours

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

实验步骤: 4-(Dimethylamino)butanol (88.5g) was added dropwise at 0° C. over 2 hours to stirred thionyl chloride (93.4 g) then the mixture was stirred at ambient temperature for 1 hour and poured into ethanol (500 ml). The stirred solution was heated under reflux for 10 minutes, then the solvent was removed in vacuo. The solid residue crystallised from ethanol as a white solid which was collected by filtration, washed with ethanol, and dried in vacuo at ambient temperature for 24 hours to give 1-chloro-4-(dimethylamino)butane hydrochloride as a white solid (115 g), m.p. 100°-105° C. The stirred solution was heated under reflux for 10 minutes the solvent was removed in vacuo The solid residue crystallised from ethanol as a white solid which was collected by filtration washed with ethanol dried in vacuo at ambient temperature for 24 hours

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-4-(dimethylamino)-butane hydrochloride (115 g), thiourea (51.9 g) and ethanol (500 ml) was heated under reflux for 24 hours then allowed to stand at 4° C. for 24 hours. The resulting solid was collected by filtration, washed with ether, and dried in vacuo at ambient temperature for 24 hours to give S-[4-(dimethylamino)butyl]isothiourea dihydrochloride as an off-white solid (140 g), m.p. 179°-182° C. was heated under reflux for 24 hours The resulting solid was collected by filtration washed with ether dried in vacuo at ambient temperature for 24 hours

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

实验步骤: 4-(Dimethylamino)butanol (88.5g) was added dropwise at 0° C. over 2 hours to stirred thionyl chloride (93.4 g) then the mixture was stirred at ambient temperature for 1 hour and poured into ethanol (500 ml). The stirred solution was heated under reflux for 10 minutes, then the solvent was removed in vacuo. The solid residue crystallised from ethanol as a white solid which was collected by filtration, washed with ethanol, and dried in vacuo at ambient temperature for 24 hours to give 1-chloro-4-(dimethylamino)butane hydrochloride as a white solid (115 g), m.p. 100°-105° C. The stirred solution was heated under reflux for 10 minutes the solvent was removed in vacuo The solid residue crystallised from ethanol as a white solid which was collected by filtration washed with ethanol dried in vacuo at ambient temperature for 24 hours