HCID 66936015, Verbindung → (4Ar,8as)-1-methyldecahydroquinoxaline

HRID 1366660Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1366660
[CH3:1][N:2]1[C@@H:11]2[C@@H:6]([CH2:7][CH2:8][CH2:9][CH2:10]2)[N:5](C(OCC2C=CC=CC=2)=O)[CH2:4][CH2:3]1>CO>[CH3:1][N:2]1[C@@H:11]2[C@@H:6]([CH2:7][CH2:8][CH2:9][CH2:10]2)[NH:5][CH2:4][CH2:3]1

Komponenten

3

Edukt 1

HCID 66936015HCID 66936015, Verbindung

Produkt 1

HCID 231577(4Ar,8as)-1-methyldecahydroquinoxalineAusbeute 144,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

Phenylmethyl (4aS,8aR)-4-methyloctahydro-1(2H)-quinoxalinecarboxylate (2.7 g, 9.4 mmol) was dissolved in 140 mL of MeOH, degassed and placed under argon. 10% Pd/C (400 mg) was added, and the contents were thoroughly degassed and placed under a hydrogen balloon for approximately 2 hrs. The contents were then degassed and filtered through Celite, and the Celite pad was washed with DCM and MeOH. After 19.6 mL 1N HCl was added, the resulting filtrate was concentrated in vacuo to provide the hydrochloride salt of (4aR,8aS)-1-methyldecahydroquinoxaline (2.1 g, 100%). LCMS: (M+H)+: 155.1.

Aufarbeitung

  1. customdegassed
  2. addition10% Pd/C (400 mg) was added
  3. customthe contents were thoroughly degassed
  4. customfor approximately 2 hrs
  5. customThe contents were then degassed
  6. filtrationfiltered through Celite
  7. washthe Celite pad was washed with DCM and MeOH
  8. additionAfter 19.6 mL 1N HCl was added
  9. concentrationthe resulting filtrate was concentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-2207c62860274943abe7e9e2ad90d50e
Quelldatensatz
uspto-grants-2011_02
Patentnummer
US07893056B2

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