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1,4-Dibenzyl-2-(methoxymethyl)piperazine → 2-(Methoxymethyl)piperazine

HRID 16873
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 16873
C([N:8]1[CH2:13][CH2:12][N:11](CC2C=CC=CC=2)[CH2:10][CH:9]1[CH2:21][O:22][CH3:23])C1C=CC=CC=1>C(O)C.[Pd]>[CH3:23][O:22][CH2:21][CH:9]1[CH2:10][NH:11][CH2:12][CH2:13][NH:8]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 1

HCID 197635561,4-Dibenzyl-2-(methoxymethyl)piperazine

Produkt 1

HCID 142302642-(Methoxymethyl)piperazineAusbeute 84,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

1,4-Dibenzyl-2-(methoxymethyl)piperazine (1.578 g, 5.08 mmol) and palladium (10% on carbon, 0.163 g, 1.53 mmol) in ethanol (50.8 ml) were stirred under an atmosphere of hydrogen at room temperature for 3 days. The reaction mixture was filtered through celite, washing with ethanol. The resulting mixture was evaporated to dryness to afford crude product. The crude product was purified by ion exchange chromatography, using a SCX column. The desired product was eluted from the column using 7M NH3/MeOH and fractions were evaporated to dryness to afford 2-(methoxymethyl)piperazine (0.559 g, 84%) as a yellow oil. This was used directly without further purification.

Aufarbeitung

  1. filtrationThe reaction mixture was filtered through celite
  2. washwashing with ethanol
  3. customThe resulting mixture was evaporated to dryness
  4. customto afford crude product
  5. customThe crude product was purified by ion exchange chromatography
  6. washThe desired product was eluted from the column
  7. customwere evaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-a5d6aecb5220441a957e5d9325a888d1
Quelldatensatz
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07737149B2

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