Reaktion #51047

Reaktionsgleichung

3-bromopropanol

N-methylpiperazine

potassium carbonate

→

1-(3-hydroxypropyl)-4-methylpiperazine

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated
2. 2
   Temperaturto reflux for 20 hours
3. 3
   Filtrationfiltered
4. 4
   SonstigeThe filtrate was evaporated
5. 5
   Sonstigethe residue was triturated under diethyl ether
6. 6
   FiltrationThe resultant mixture was filtered
7. 7
   Sonstigethe filtrate was evaporated
8. 8
   workup.DISTILLATIONThe residue was purified by distillation at about 60-70° C. under about 0.2 mm Hg

Vorschrift

A mixture of 3-bromopropanol (20 ml), N-methylpiperazine (29 ml), potassium carbonate (83 g) and ethanol (200 ml)was stirred and heated to reflux for 20 hours. The mixture was cooled to ambient temperature and filtered. The filtrate was evaporated and the residue was triturated under diethyl ether. The resultant mixture was filtered and the filtrate was evaporated. The residue was purified by distillation at about 60-70° C. under about 0.2 mm Hg to give 1-(3-hydroxypropyl)-4-methylpiperazine (17 g); NMR Spectrum: (CDCl3) 1.72 (m, 2H), 2.3 (s, 3H), 2.2-2.8 (m, 8H), 2.6 (t, 2H), 3.8 (t, 2H), 5.3 (br s, 1H).

Quelle