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Piperazine → 2-Methyl-1-(piperazin-1-yl)propan-2-ol

HRID 2389283
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2389283
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.Cl[CH2:8][C:9]([CH3:12])([OH:11])[CH3:10]>C(O)C>[CH3:8][C:9]([OH:11])([CH3:12])[CH2:10][N:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 4837PiperazineHCID 684091-Chloro-2-methylpropan-2-ol

Produkt 1

HCID 2582022-Methyl-1-(piperazin-1-yl)propan-2-olAusbeute 60 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

piperazine (6.88 g, 80.0 mmol) was dissolved in ethanol (40 mL), and 1-chloro-2-methyl-2-propanol (2.18 g, 20.0 mmol) was added thereto, and then, the mixture was stirred at 110° C. for 6 hours. After the mixture was left to cool to room temperature, the solvent was evaporated. Then, ethyl acetate was added to the residue, and the precipitated solid was removed by filtration. The solvent of the filtrate was removed under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/methanol=90/10) to give 2-methyl-1-(piperazin-1-yl)propan-2-ol (1.89 g, 11.96 mmol, 60%).

Aufarbeitung

  1. waitAfter the mixture was left
  2. temperatureto cool to room temperature
  3. customthe solvent was evaporated
  4. additionThen, ethyl acetate was added to the residue
  5. customthe precipitated solid was removed by filtration
  6. customThe solvent of the filtrate was removed under reduced pressure
  7. customthe residue was purified by silica gel column chromatography (ethyl acetate/methanol=90/10)

Quellen und Nachweise

ORD-Eintrag
ord-a6bc1f669c0746ee8b14d1feff500d20
Quelldatensatz
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08273738B2

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