Potassium Carbonate → 3-(4-Methyl-1-piperazine)propan-1-ol

HRID 22769

Reaktionsgleichung

Reaktionsgleichung von HRID 22769
Br[CH2:2][CH2:3][CH2:4][OH:5].[CH3:6][N:7]1[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]1.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[OH:5][CH2:4][CH2:3][CH2:2][N:10]1[CH2:11][CH2:12][N:7]([CH3:6])[CH2:8][CH2:9]1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 123083-Bromo-1-propanolHCID 531671-Methylpiperazine

Produkt 1

HCID 792083-(4-Methyl-1-piperazine)propan-1-ol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

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).

Aufarbeitung

  1. temperatureheated
  2. temperatureto reflux for 20 hours
  3. filtrationfiltered
  4. customThe filtrate was evaporated
  5. customthe residue was triturated under diethyl ether
  6. filtrationThe resultant mixture was filtered
  7. customthe filtrate was evaporated
  8. distillationThe residue was purified by distillation at about 60-70° C. under about 0.2 mm Hg

Quellen und Nachweise

ORD-Eintrag
ord-8cae2a34954640a9b6a0abd424a54f32
Quelldatensatz
uspto-grants-2005_02
Patentnummer
US06849625B2

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