2-[2-(dimethylamino)ethyldisulfanyl]-N,N-dimethylethanamine

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

Procedure: In a 100 ml round-bottom flask, 8.5 g of N,N-dimethyl-2-chloroethylamine hydrochloride, 8.7 g of sodium thiosulfate and 50 ml of distilled water were charged and heated under reflux for 2 hours. 36% hydrochloric acid (5.1 g) was added, and the mixture was further heated under reflux for 1 hour. With cooling the mixture on an ice bath, 5.5 g of sodium hydroxide was slowly added to make the mixture alkaline, which was then subjected to extraction twice with 50 ml of ethyl acetate. After desiccating with anhydrous potassium carbonate, the solvent was removed by distillation and distilled under reduced pressure to give 7.0 g of bis(N,N-dimethyl-2-aminoethyl)disulfide, the precursor. heated under reflux for 2 hours the mixture was further heated under reflux for 1 hour With cooling the mixture on an ice bath was then subjected to extraction twice with 50 ml of ethyl acetate the solvent was removed by distillation distilled under reduced pressure

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

Procedure: In a 100 ml round-bottom flask, 8.5 g of N,N-dimethyl-2-chloroethylamine hydrochloride, 8.7 g of sodium thiosulfate and 50 ml of distilled water were charged and heated under reflux for 2 hours. 36% hydrochloric acid (5.1 g) was added, and the mixture was further heated under reflux for 1 hour. With cooling the mixture on an ice bath, 5.5 g of sodium hydroxide was slowly added to make the mixture alkaline, which was then subjected to extraction twice with 50 ml of ethyl acetate. After desiccating with anhydrous potassium carbonate, the solvent was removed by distillation and distilled under reduced pressure to give 7.0 g of bis(N,N-dimethyl-2-aminoethyl)disulfide, the precursor. heated under reflux for 2 hours the mixture was further heated under reflux for 1 hour With cooling the mixture on an ice bath was then subjected to extraction twice with 50 ml of ethyl acetate the solvent was removed by distillation distilled under reduced pressure

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

Procedure: In a 100 ml round-bottom flask, 8.5 g of N,N-dimethyl-2-chloroethylamine hydrochloride, 8.7 g of sodium thiosulfate and 50 ml of distilled water were charged and heated under reflux for 2 hours. 36% hydrochloric acid (5.1 g) was added, and the mixture was further heated under reflux for 1 hour. With cooling the mixture on an ice bath, 5.5 g of sodium hydroxide was slowly added to make the mixture alkaline, which was then subjected to extraction twice with 50 ml of ethyl acetate. After desiccating with anhydrous potassium carbonate, the solvent was removed by distillation and distilled under reduced pressure to give 7.0 g of bis(N,N-dimethyl-2-aminoethyl)disulfide, the precursor. heated under reflux for 2 hours the mixture was further heated under reflux for 1 hour With cooling the mixture on an ice bath was then subjected to extraction twice with 50 ml of ethyl acetate the solvent was removed by distillation distilled under reduced pressure