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Tert-butyl(4-benzylpiperazin-1-yl)carbamate → tert-Butyl piperazin-1-ylcarbamate

HRID 856033
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 856033
[C:1]([O:5][C:6](=[O:21])[NH:7][N:8]1[CH2:13][CH2:12][N:11](CC2C=CC=CC=2)[CH2:10][CH2:9]1)([CH3:4])([CH3:3])[CH3:2].[H][H]>C(O)C.[OH-].[OH-].[Pd+2]>[N:8]1([NH:7][C:6](=[O:21])[O:5][C:1]([CH3:3])([CH3:2])[CH3:4])[CH2:9][CH2:10][NH:11][CH2:12][CH2:13]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 23081385Tert-butyl(4-benzylpiperazin-1-yl)carbamateHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 21701658tert-Butyl piperazin-1-ylcarbamateAusbeute 99 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 9942167Palladium hydroxideKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

Tert-butyl(4-benzylpiperazin-1-yl)carbamate (42.22 g, 145 mmol) prepared in Reference Example 35 was dissolved in ethanol (300 ml). To which 20% palladium hydroxide/carbon (6.0 g) was added, and the mixture was stirred at room temperature under an atmospheric pressure of hydrogen for 20 minutes, and then at 50° C. for 30 minutes. The catalyst was removed by filtration, and the filtrate was concentrated under reduced pressure. Thus obtained solid was washed with IPE, collected by filtration, and dried under reduced pressure to afford tert-butyl piperazin-1-yl-carbamate (28.9 g, yield 99%) as a colorless crystalline powder.

Aufarbeitung

  1. customThe catalyst was removed by filtration
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. washThus obtained solid was washed with IPE
  4. filtrationcollected by filtration
  5. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-88382c786981466c9830c93761e911bd
Quelldatensatz
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07262212B2

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