反应详情

Agitated in a reaction vessel are 256 parts of N,N'-bis(2,2-dimethyl-3-aminopropyl)piperazine with 400 parts of O-octyl carbamate and 130 parts of n-octanol at a reflux temperature of 190° C.-200° C. for 1 hour while the ammonia is removed by distillation. At that point, an additional 650 parts of n-octanol are allowed to flow into the reaction mixture and the reaction is continued at reflux temperature for 7 hours. Unreacted octanol and O-octylcarbonate are removed by distillation up to a sump temperature of 180° C.-200° C. at 2 millibars. By transcrystallization of the residue from acetone/water, 506 parts of N,N'-bis(octoxycarbonylaminoneopentyl)piperazine, C32H64N4O4 (molecular weight 568), are obtained corresponding with 89 percent of theory relative to N,N'-bis(2,2-dimethyl-3-aminopropyl)piperaxine. The melting point is 66° C.-68° C.

1. customat a reflux temperature of 190° C.-200° C.
2. customfor 1 hour
3. customis removed by distillation
4. temperatureat reflux temperature for 7 hours
5. customare removed by distillation up to a sump temperature of 180° C.-200° C. at 2 millibars