1-Oxaspiro[5.5]undec-3-ene, 4-methyl- → HCID 3764775, Verbindung

HRID 716491Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 716491
[CH3:1][C:2]1[CH2:7][C:6]2([CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]2)[O:5][CH2:4][CH:3]=1.[H][H]>[Ni].C(O)(C)C>[CH3:1][CH:2]1[CH2:7][C:6]2([CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]2)[O:5][CH2:4][CH2:3]1

Komponenten

5

Edukt 2

HCID 111164241-Oxaspiro[5.5]undec-3-ene, 4-methyl-HCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 3764775HCID 3764775, VerbindungAusbeute 93 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 935NickelKatalysatorHCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

A solution of 4-methyl-1-oxaspiro[5.5]undec-3-ene (1.66 kg, 10.0 mols), isopropyl alcohol (100 ml) and Raney nickel (100 g) or other suitable sponge-metal catalyst was hydrogenated at 400 psi, at 140° C. for 10-12 h until the theoretical amount of hydrogen was taken up. The mixture was cooled and filtrated. The isopropyl alcohol was evaporated and the residue obtained was distilled under reduced pressure to provide 4-methyl-1-oxaspiro [5.5] undecane (1.56 kg, yield: 93%, purity: 99% sum of the isomers).

Aufarbeitung

  1. temperatureThe mixture was cooled
  2. filtrationfiltrated
  3. customThe isopropyl alcohol was evaporated
  4. customthe residue obtained
  5. distillationwas distilled under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-ce2c954baa4f4245bddaef47eff299fb
Quelldatensatz
uspto-grants-2015_11
Patentnummer
US09187709B2

Notizen zur Reaktion

Wird geladen…