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(1,4-Dibenzylpiperazin-2-yl)-N,N-dimethylmethanamine → N,N-dimethyl-2-piperazinemethanamine

HRID 248456
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 248456
[CH3:1][N:2]([CH2:4][CH:5]1[CH2:10][N:9](CC2C=CC=CC=2)[CH2:8][CH2:7][N:6]1CC1C=CC=CC=1)[CH3:3]>C(O)C.C1CCCCC1.C(O)(=O)C.[Pd]>[CH3:1][N:2]([CH3:3])[CH2:4][CH:5]1[CH2:10][NH:9][CH2:8][CH2:7][NH:6]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 1

HCID 14664170(1,4-Dibenzylpiperazin-2-yl)-N,N-dimethylmethanamine

Produkt 1

HCID 14664185N,N-dimethyl-2-piperazinemethanamine

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 23938PalladiumKatalysatorHCID 176Acetic AcidLösungsmittelHCID 702EthanolLösungsmittelHCID 8078
Cyclohexane
Lösungsmittel

Versuchsvorschrift

A 4.7 g portion of 2-dimethylaminomethyl-1,4-bis(phenylmethyl)piperazine was dissolved in a mixture of 50 ml of ethanol, 20 ml of cyclohexane and 10 ml of glacial acetic acid. A 2.0 g portion of 10% palladium on carbon was added, the mixture was refluxed overnight and then filtered. The filtrate was evaporated, 5 ml of saturated aqueous potassium bicarbonate was added to the residue and this was extracted several times with dichloromethane. The extracts were combined, dried, filtered and evaporated, giving a gum which solidified on standing, giving 1.02 g of N,N-dimethyl-2-piperazinemethanamine.

Aufarbeitung

  1. temperaturethe mixture was refluxed overnight
  2. filtrationfiltered
  3. customThe filtrate was evaporated
  4. addition5 ml of saturated aqueous potassium bicarbonate was added to the residue
  5. extractionthis was extracted several times with dichloromethane
  6. customdried
  7. filtrationfiltered
  8. customevaporated
  9. customgiving a gum which

Quellen und Nachweise

ORD-Eintrag
ord-f962c2fba81642c2a6d4365241e98f34
Quelldatensatz
uspto-grants-1993_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05210193

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