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

HRID 435162Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 435162
[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-8598290cbe14487b992bd048832a7430
Quelldatensatz
uspto-grants-1983_08
Patentnummer
US04400512

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