propyl N-[3-(dimethylamino)propyl]carbamate;hydrochloride

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

Procedure: A solution of phosphorous acid (2.87 g in water (50 ml)) was stirred for 1 hour with a solution of sodium hydroxide (2.8 g in water (50 ml)). Propyl 3-(dimethyiamino)propylcarbamate hydrochloride (15.7 g) in water (50 ml) was added and the mixture stirred for 30 min, evaporated to dryness, dichloromethane (450 ml) added and re-evaporated. The residue was dissolved in dichloromethane (150 ml) allowed to stand for 1 hour and the insoluble white solid (sodium chloride) filtered off. The filtrate was evaporated to leave dimethyl-[3-(propoxycarbonylamino)propyl]ammonium phosphite, as a viscous colorless oil. evaporated to dryness, dichloromethane (450 ml) added re-evaporated The residue was dissolved in dichloromethane (150 ml) to stand for 1 hour the insoluble white solid (sodium chloride) filtered off The filtrate was evaporated

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

Procedure: A solution of phosphorous acid (2.87 g in water (50 ml)) was stirred for 1 hour with a solution of sodium hydroxide (2.8 g in water (50 ml)). Propyl 3-(dimethyiamino)propylcarbamate hydrochloride (15.7 g) in water (50 ml) was added and the mixture stirred for 30 min, evaporated to dryness, dichloromethane (450 ml) added and re-evaporated. The residue was dissolved in dichloromethane (150 ml) allowed to stand for 1 hour and the insoluble white solid (sodium chloride) filtered off. The filtrate was evaporated to leave dimethyl-[3-(propoxycarbonylamino)propyl]ammonium phosphite, as a viscous colorless oil. evaporated to dryness, dichloromethane (450 ml) added re-evaporated The residue was dissolved in dichloromethane (150 ml) to stand for 1 hour the insoluble white solid (sodium chloride) filtered off The filtrate was evaporated