2-Azaspiro[5.5]undec-1-ene → 2-Azaspiro[5.5]undecane

HRID 1995637Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1995637
[CH:1]1[C:6]2([CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]2)[CH2:5][CH2:4][CH2:3][N:2]=1.[H][H]>[Ni].C(O)C>[CH2:1]1[C:6]2([CH2:7][CH2:8][CH2:9][CH2:10][CH2:11]2)[CH2:5][CH2:4][CH2:3][NH:2]1

Komponenten

5

Edukt 2

HCID 18835922-Azaspiro[5.5]undec-1-eneHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 50061172-Azaspiro[5.5]undecaneAusbeute 88,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 935NickelKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of 2-azaspiro[5.5]-undec-1-ene (15 g.; 0.10 mole) and one teaspoon (3 g.) of W2 Raney nickel catalyst in absolute ethanol (300 ml.) is hydrogenated at an initial pressure of 40 psi until hydrogen uptake ceases (2 hours). The mixture is filtered through celite and the filtrate concentrated under reduced pressure. Distillation of the residual liquid yields 88% of 2-azaspiro-[5.5]-undecane (13.5 g.), b.p. 55°-57° C./0.10 mm.

Aufarbeitung

  1. filtrationThe mixture is filtered through celite
  2. concentrationthe filtrate concentrated under reduced pressure
  3. distillationDistillation of the residual liquid

Quellen und Nachweise

ORD-Eintrag
ord-40f1904dd9f9455ab5f8769b906c3944
Quelldatensatz
uspto-grants-1983_09
Patentnummer
US04405630

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