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HCID 66936334, Verbindung → HCID 55288067, Verbindung

HRID 1366648
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Reaktionsgleichung

Reaktionsgleichung von HRID 1366648
[CH3:1][N:2]1[CH2:7][C@@H:6]([CH3:8])[N:5](CC2C=CC=CC=2)[CH2:4][C@H:3]1[CH3:16]>CO>[CH3:1][N:2]1[CH2:7][C@@H:6]([CH3:8])[NH:5][CH2:4][C@H:3]1[CH3:16]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 1

HCID 66936334HCID 66936334, Verbindung

Produkt 1

HCID 55288067HCID 55288067, VerbindungAusbeute 100 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

(2R,5R)-1,2,5-Trimethyl-4-(phenylmethyl)piperazine (680 mg, 3.11 mmol) was dissolved in 50 mL of MeOH, degassed and placed under argon. 10% Pd/C (170 mg) was added, and the contents were thoroughly degassed and placed under a hydrogen balloon for approximately 3 hrs. The contents were then degassed and filtered through Celite, and the Celite pad was washed with DCM and MeOH. After 6.5 mL 1N HCl was added, the resulting filtrate was concentrated in vacuo to provide the hydrochloride salt of (2R,5R)-1,2,5-trimethylpiperazine (251 mg, 100%). LCMS: (M+H)+: 129.1.

Aufarbeitung

  1. custom
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degassed
  • addition10% Pd/C (170 mg) was added
  • customthe contents were thoroughly degassed
  • customfor approximately 3 hrs
  • customThe contents were then degassed
  • filtrationfiltered through Celite
  • washthe Celite pad was washed with DCM and MeOH
  • additionAfter 6.5 mL 1N HCl was added
  • concentrationthe resulting filtrate was concentrated in vacuo
  • Quellen und Nachweise

    ORD-Eintrag
    ord-0025c7cdb0af4412abb76d77aa9f27b8
    Quelldatensatz
    uspto-grants-2011_02
    DOI
    10.6084/m9.figshare.5104873.v1
    Patentnummer
    US07893056B2

    Notizen zur Reaktion

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