Piperazine → HCID 22665942, compound

Participants

Reaction Conditions

Reaction Steps

Into a round bottom flask equipped with stirrer, thermometer, dropping funnel and reflux condenser were weighed 154.8 g (1.8 mole) of piperazine and 69.6 g (0.8 mole) of morpholine and 220 ml of water. After a clear solution at 40° C. was obtained, the solution was heated to 55-65° C. and with vigorous stirring 185 g (2 mole) of epichlorohydrin were added at such a rate, that the temperature did not exceed 80° C. After all the epichlorohydrin had been added the reaction mixture was heated to 85° C. until all of the alkylating agents had been consumed (negative Preussmann test after 4 hours). 108.8 g (0.68 mole) of 25% NaOH and 40 g of water were added and the reaction mixture was stirred for another hour at 85° C. Then additional 47 g of water were added and the mixture was allowed to cool to room temperature. 233.6 g (equivalent to 1,292 mole oxidizable nitrogen atoms) were mixed with 22.1 g (0.276) of 50% NaOH and then heated to 55-65° C. At that temperature 102.4 g (1,421 mole) of H202 (47.2%) were added dropwise over a period of 3.5 hours. After the addition was completed, the reaction mixture was heated held at the same temperature for 3 more hours and was then stirred at room temperature overnight. Pt/C was added, unreacted H202 destroyed and the solution then filtered.

Provenance & Evidence