Reaktion #1500897

Reaktionsgleichung

hydrogen chloride

N,N'-dibenzylethylenediamine

ethyl chloroacetate

sodium carbonate

→

1,4-Bis(phenylmethyl)piperazinone, hydrochloride

Lösungsmittel

isopropanol

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturis heated
2. 2
   Temperaturunder reflux for 20 hours
3. 3
   SonstigeThe ethanol is removed under reduced pressure
4. 4
   Sonstigethe residue is partitioned between chloroform and water
5. 5
   SonstigeEvaporation of the chloroform
6. 6
   Sonstigegives an oil which
7. 7
   FiltrationThe precipitate of 1,4-bis(phenylmethyl)piperazinone hydrochloride is filtered off
8. 8
   Sonstigerecrystallized from isopropanol, m.p. 209°-212°

Vorschrift

A mixture of N,N'-dibenzylethylenediamine (24.0 g., 0.1 mole), ethyl chloroacetate (V, 24.51 g., 0.2 mole), anhydrous sodium carbonate (10 g., 0.094 mole) in ethanol (250 ml.) is heated under reflux for 20 hours. The ethanol is removed under reduced pressure and the residue is partitioned between chloroform and water. Evaporation of the chloroform gives an oil which is dissolved in isopropanol (200 ml.) and acidified with ethereal hydrogen chloride. The precipitate of 1,4-bis(phenylmethyl)piperazinone hydrochloride is filtered off and recrystallized from isopropanol, m.p. 209°-212°.

Quelle