2-Methyl-3-phenyl-1-propanol → 3-Cyclohexyl-2-methylpropan-1-ol
Reaktionsgleichung
[CH3:1][CH:2]([CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[CH2:3][OH:4]>[Ni].O>[CH3:1][CH:2]([CH2:5][CH:6]1[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1)[CH2:3][OH:4]Komponenten
4
Edukt 1
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
2-Methyl-3-phenylpropanol (219 g., 1.46 mol.) and 10.30 g. of 50% Ni on silica catalyst (4.7 wt %, G-49-C, United Catalyst) were stirred at 700 rpm in a Parr reactor at 150° C. and 200-600 psi of hydrogen until hydrogen absorption stopped (12 hours). Utilizing 2 wt. % of the catalyst requires that the reaction be run at 180° C. The reaction mixture was filtered through a filter bed (Celite™) using toluene as a rinse solvent and concentrated to a clear, colorless liquid. The odor grade product was isolated by fractional distillation, 174 g., 80% yield; bp 80° C. at 4 mm. Odor: very pleasant green, fruity, rosy. Mass Spectrum from 5508-36. MS (El) m/z (relative intensity) 138 (M+−H2O, 15), 123 (M+−Me and H2O, 15).
Aufarbeitung
- custom200-600 psi of hydrogen until hydrogen absorption
- custom(12 hours)
- custombe run at 180° C
- filtrationThe reaction mixture was filtered through a filter bed (Celite™)
- concentrationconcentrated to a clear, colorless liquid
- customThe odor grade product was isolated by fractional distillation, 174 g
Quellen und Nachweise
- ORD-Eintrag
- ord-d26212e3fd26489c9ec90030009ce022
- Quelldatensatz
- uspto-grants-2001_02
- Patentnummer
- US06187727B1
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